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_4066697
_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            'C15 H25 Cl2 N3 O2 P Rh S'
_chemical_formula_weight         516.22
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.221(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3140(3)
_cell_length_b                   7.2646(2)
_cell_length_c                   25.8648(9)
_cell_measurement_reflns_used    6456
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.332
_cell_measurement_theta_min      2.9067
_cell_volume                     1937.53(10)
_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 0.848
_diffrn_measurement_details
;
 1 omega 47.00 90.00 1.0000 32.0000
 omega____ theta____ kappa____ phi______ frames
 - 17.8225 37.0000 -120.0000 43
 2 omega -48.00 3.00 1.0000 32.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 115.0000 167.0000 51
 3 omega -43.00 46.00 1.0000 32.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 77.0000 120.0000 89
 4 omega -87.00 10.00 1.0000 32.0000
 omega____ theta____ kappa____ phi______ frames
 - -19.5412 -77.0000 0.0000 97
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0556428
_diffrn_orient_matrix_UB_12      0.0520975
_diffrn_orient_matrix_UB_13      0.0062892
_diffrn_orient_matrix_UB_21      0.030724
_diffrn_orient_matrix_UB_22      0.0810784
_diffrn_orient_matrix_UB_23      -0.0088799
_diffrn_orient_matrix_UB_31      -0.0263255
_diffrn_orient_matrix_UB_32      -0.0156473
_diffrn_orient_matrix_UB_33      -0.0251746
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            10661
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         29.40
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    1.363
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.90785
_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    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         4531
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0312P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                3815
_reflns_number_total             4531
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100579e_si_001.cif
_cod_data_source_block           FM443A_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_database_code               4066697