Taming functionality: easy-to-handle chiral phosphiranes
Arne Ficks; Ivan Martinez-Botella; Beverly Stewart; Ross W. Harrington; William Clegg; Lee J. Higham; Chem.Commun. 47 (2011) 8274–; doi:10.1039/c1cc12440d

data_7106680
_publ_section_title
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 Taming functionality: easy-to-handle chiral phosphiranes
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_journal_name_full               Chem.Commun.
_journal_page_first              8274
_journal_paper_doi               10.1039/c1cc12440d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C46 H38 Cl2 O2 P2 Pt, C H Cl3'
_chemical_formula_sum            'C47 H39 Cl5 O2 P2 Pt'
_chemical_formula_weight         1070.06
_chemical_name_systematic
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?
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_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 122.417(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   19.9049(8)
_cell_length_b                   8.3739(2)
_cell_length_c                   14.7846(6)
_cell_measurement_reflns_used    6551
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.40
_cell_measurement_theta_min      2.81
_cell_volume                     2080.30(17)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Oxford Diffraction Gemini A Ultra diffractometer'
_diffrn_measurement_method       'thick-slice \w scans'
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8694
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    3.811
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.619
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3631
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                3587
_reflns_number_total             3631
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1cc12440d.txt
_cod_data_source_block           ljh12_compound_4b
_cod_original_cell_volume        2080.30(13)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7106680
_computing_special_details
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TITL ljh12 in C2
CELL 0.71073 19.9049 8.3739 14.7846 90.000 122.417 90.000
ZERR 2.00 0.0008 0.0002 0.0006 0.000 0.005 0.000
LATT -7
SYMM -X,Y,-Z
SFAC C H O P CL PT
UNIT 94 78 4 4 10 2
TEMP -123

REM one chloroform squeezed per molecule

L.S. 8
BOND $H
CONF

REM yellow plate
SIZE 0.08 0.08 0.02

FMAP 2
PLAN 5
OMIT 0 0 2
OMIT -2 0 2

ACTA 52

REM EXTI 0.000000
WGHT 0.040000
FVAR 3.22058
PT 6 0.500000 0.438783 0.500000 10.50000 0.01781 0.01372 =
0.01757 0.00000 0.00860 0.00000
CL 5 0.402621 0.242084 0.411066 11.00000 0.03955 0.02111 =
0.03928 -0.00250 0.01214 -0.01163
P 4 0.410254 0.613334 0.389988 11.00000 0.01623 0.01701 =
0.01954 -0.00126 0.00861 0.00130
O 3 0.404994 0.965996 0.205300 11.00000 0.02130 0.01858 =
0.04779 0.00384 0.01139 0.00151
C1 1 0.393220 0.815455 0.414009 11.00000 0.03221 0.01852 =
0.03130 -0.00587 0.01753 0.00210
AFIX 23
H1A 2 0.428145 0.857737 0.487535 11.00000 -1.20000
H1B 2 0.379024 0.894510 0.356661 11.00000 -1.20000
AFIX 0
C2 1 0.328079 0.694290 0.395329 11.00000 0.01966 0.03330 =
0.03172 0.00563 0.01627 0.01264
AFIX 23
H2A 2 0.275842 0.702098 0.326973 11.00000 -1.20000
H2B 2 0.324993 0.665302 0.457925 11.00000 -1.20000
AFIX 0
C3 1 0.372942 0.583658 0.250001 11.00000 0.00888 0.01221 =
0.01611 0.00052 0.00420 0.00223
C4 1 0.303809 0.489323 0.191052 11.00000 0.01580 0.01994 =
0.02354 0.00188 0.00750 0.00061
AFIX 43
H4 2 0.277388 0.451638 0.224629 11.00000 -1.20000
AFIX 0
C5 1 0.274691 0.451876 0.087635 11.00000 0.02062 0.01817 =
0.02744 -0.00424 0.00830 -0.00474
AFIX 43
H5 2 0.228230 0.387704 0.049684 11.00000 -1.20000
AFIX 0
C6 1 0.312133 0.506495 0.034828 11.00000 0.01290 0.03259 =
0.02313 -0.00366 0.00744 0.00387
C7 1 0.284172 0.465164 -0.072018 11.00000 0.02555 0.04939 =
0.02795 -0.01326 0.01061 0.00322
AFIX 43
H7 2 0.241381 0.391604 -0.108173 11.00000 -1.20000
AFIX 0
C8 1 0.316373 0.526944 -0.124189 11.00000 0.03035 0.09365 =
0.02586 -0.01775 0.01123 0.00305
AFIX 43
H8 2 0.294856 0.501412 -0.197353 11.00000 -1.20000
AFIX 0
C9 1 0.381913 0.629272 -0.069784 11.00000 0.04409 0.06894 =
0.04350 0.00299 0.03386 0.00430
AFIX 43
H9 2 0.405066 0.672096 -0.106442 11.00000 -1.20000
AFIX 0
C10 1 0.413567 0.669153 0.036354 11.00000 0.02189 0.05206 =
0.02423 0.00620 0.01163 0.00193
AFIX 43
H10 2 0.458111 0.738701 0.072268 11.00000 -1.20000
AFIX 0
C11 1 0.379439 0.606178 0.090697 11.00000 0.01714 0.03429 =
0.01943 0.00119 0.00874 0.01203
C12 1 0.411698 0.644376 0.202781 11.00000 0.01403 0.01610 =
0.02157 0.00001 0.00733 0.00566
C13 1 0.485405 0.741406 0.259447 11.00000 0.01288 0.02849 =
0.01643 0.00078 0.00726 0.00006
C14 1 0.562971 0.668541 0.307733 11.00000 0.01632 0.03321 =
0.01374 0.00225 0.01011 0.00321
C15 1 0.572468 0.500837 0.315586 11.00000 0.01618 0.03163 =
0.03304 0.00563 0.01124 0.00733
AFIX 43
H15 2 0.527496 0.433722 0.291573 11.00000 -1.20000
AFIX 0
C16 1 0.647050 0.434410 0.358127 11.00000 0.02572 0.03456 =
0.03721 0.00818 0.01376 0.01430
AFIX 43
H16 2 0.653298 0.321705 0.364493 11.00000 -1.20000
AFIX 0
C17 1 0.713455 0.532074 0.391904 11.00000 0.01404 0.05711 =
0.02689 -0.00516 0.00981 0.00772
AFIX 43
H17 2 0.764216 0.484886 0.419250 11.00000 -1.20000
AFIX 0
C18 1 0.706029 0.696136 0.385935 11.00000 0.01305 0.05454 =
0.01379 -0.00632 0.00511 -0.00332
AFIX 43
H18 2 0.751605 0.761405 0.409926 11.00000 -1.20000
AFIX 0
C19 1 0.630912 0.766540 0.344293 11.00000 0.01915 0.03713 =
0.01579 0.00089 0.01110 0.00005
C20 1 0.621411 0.934110 0.340347 11.00000 0.01754 0.03550 =
0.02909 0.01088 0.00735 -0.00409
AFIX 43
H20 2 0.666814 1.000777 0.366769 11.00000 -1.20000
AFIX 0
C21 1 0.548966 1.001547 0.299704 11.00000 0.03232 0.02245 =
0.04155 0.00139 0.01672 -0.00608
AFIX 43
H21 2 0.544474 1.114345 0.301057 11.00000 -1.20000
AFIX 0
C22 1 0.480007 0.905798 0.255316 11.00000 0.01867 0.02047 =
0.02517 0.00650 0.01000 0.00390
C23 1 0.395605 1.133004 0.179530 11.00000 0.03811 0.01981 =
0.05828 0.01025 0.02352 0.01028
AFIX 137
H23A 2 0.338944 1.160652 0.139883 11.00000 -1.50000
H23B 2 0.417468 1.156727 0.135346 11.00000 -1.50000
H23C 2 0.423991 1.195679 0.245764 11.00000 -1.50000

HKLF 4

REM ljh12 in C2
REM R1 = 0.0336 for 3587 Fo > 4sig(Fo) and 0.0339 for all 3631 data
REM 241 parameters refined using 1 restraints

END

WGHT 0.0400 0.0000
REM Highest difference peak 1.619, deepest hole -0.815, 1-sigma level 0.124
Q1 1 0.5087 0.4559 0.4398 11.00000 0.05 1.47
Q2 1 0.4803 0.5612 0.4862 11.00000 0.05 1.09
Q3 1 0.4767 0.3166 0.4889 11.00000 0.05 1.07
Q4 1 0.4721 0.5396 0.4286 11.00000 0.05 0.69
Q5 1 0.4699 0.3369 0.4287 11.00000 0.05 0.67
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