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_4066701
_publ_section_title
;
 2-Thia-1,3,5-triaza-7-phosphaadamantane-2,2-dioxide Revisited:
 Computational and Experimental Studies of a Neglected Phosphine
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_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            'C15 H24 Cl2 N3 O2 P Ru S'
_chemical_formula_weight         513.38
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 119.812(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.692(2)
_cell_length_b                   6.6083(3)
_cell_length_c                   23.5466(18)
_cell_measurement_reflns_used    2939
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.4127
_cell_measurement_theta_min      2.9851
_cell_volume                     3873.7(6)
_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 0.844
_diffrn_measurement_details
;
 1 omega 28.00 54.00 1.0000 148.0000
 omega____ theta____ kappa____ phi______ frames
 - 17.9787 77.0000 60.0000 26
 2 omega -38.00 37.00 1.0000 148.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.6975 37.0000 -120.0000 75
 3 omega -92.00 -59.00 1.0000 148.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.6975 179.0000 30.0000 33
 4 omega -83.00 26.00 1.0000 148.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.6975 0.0000 -150.0000 109
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0040696
_diffrn_orient_matrix_UB_12      0.0076538
_diffrn_orient_matrix_UB_13      -0.0273093
_diffrn_orient_matrix_UB_21      0.0233813
_diffrn_orient_matrix_UB_22      -0.0604903
_diffrn_orient_matrix_UB_23      0.0165312
_diffrn_orient_matrix_UB_31      -0.015696
_diffrn_orient_matrix_UB_32      -0.0883416
_diffrn_orient_matrix_UB_33      -0.013691
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.1075
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9192
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         29.48
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.96757
_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_primary    orange
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.825
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4539
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0218P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0639
_reflns_number_gt                2887
_reflns_number_total             4539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100579e_si_001.cif
_cod_data_source_block           FMRUPTASO2
_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        3873.8(4)
_cod_database_code               4066701