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_7106679
_publ_section_title
;
 Taming functionality: easy-to-handle chiral phosphiranes
;
_journal_name_full               Chem.Commun.
_journal_page_first              8274
_journal_paper_doi               10.1039/c1cc12440d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C44 H34 Cl2 P2 Pt, 0.75 C H2 Cl2'
_chemical_formula_sum            'C44.75 H35.5 Cl3.5 P2 Pt'
_chemical_formula_weight         954.34
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 105.640(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.8961(3)
_cell_length_b                   8.09268(12)
_cell_length_c                   16.9803(3)
_cell_measurement_reflns_used    9143
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      2.80
_cell_volume                     1971.17(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    '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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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 Ultra optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11728
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    3.909
_exptl_absorpt_correction_T_max  .696
_exptl_absorpt_correction_T_min  .441
_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            colourless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             943
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         2.000
_refine_diff_density_min         -0.870
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6013
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0566P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                5534
_reflns_number_total             6013
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1cc12440d.txt
_cod_data_source_block           ljh48_compound_4a
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C44.75 H35.50 Cl3.50 P2 Pt'
_cod_database_code               7106679
_computing_special_details
;
TITL ljh48 in P2(1)
CELL 0.71073 14.8961 8.09268 16.9803 90.000 105.640 90.000
ZERR 2.00 0.0003 0.00012 0.0003 0.000 0.002 0.000
LATT -1
SYMM -X,1/2+Y,-Z
SFAC C H P CL PT
UNIT 89.5 71 4 7 2
TEMP -123

ACTA

L.S. 8
FMAP 2
BOND $H
CONF
REM colourless slab
SIZE 0.25 0.20 0.10

OMIT -3 50

PLAN 5
REM EXTI 0.000000
WGHT 0.056600
FVAR 0.14604
PT 5 0.256975 0.247278 0.237762 11.00000 0.01520 0.01444 =
0.01584 0.00166 0.00230 0.00006
CL1 4 0.242640 0.015946 0.315813 11.00000 0.04634 0.01856 =
0.03541 0.01037 0.01664 0.00111
CL2 4 0.281622 0.076932 0.134659 11.00000 0.04797 0.01976 =
0.02629 -0.00626 0.01213 0.00283
P1 3 0.272731 0.454179 0.157368 11.00000 0.01363 0.01930 =
0.01528 0.00462 0.00130 0.00040
P2 3 0.232026 0.399053 0.337936 11.00000 0.01457 0.01981 =
0.01183 0.00092 0.00117 -0.00023
C1 1 0.373797 0.457970 0.117079 11.00000 0.01685 0.02110 =
0.01996 0.00211 0.00518 0.00144
C2 1 0.362814 0.381306 0.039573 11.00000 0.02462 0.03174 =
0.01375 -0.00053 0.00243 -0.00139
AFIX 43
H2A 2 0.303430 0.340628 0.010117 11.00000 -1.20000
AFIX 0
C3 1 0.436041 0.366022 0.007690 11.00000 0.03751 0.03658 =
0.01694 -0.00517 0.00956 -0.00161
AFIX 43
H3A 2 0.427374 0.315061 -0.044225 11.00000 -1.20000
AFIX 0
C4 1 0.526135 0.424779 0.050313 11.00000 0.02502 0.03486 =
0.01511 -0.00104 0.00654 0.00016
C5 1 0.602937 0.409134 0.019429 11.00000 0.03319 0.05985 =
0.02159 0.00237 0.01016 0.00704
AFIX 43
H5A 2 0.595648 0.353975 -0.031296 11.00000 -1.20000
AFIX 0
C6 1 0.687871 0.469522 0.058865 11.00000 0.02410 0.06963 =
0.03200 0.00502 0.01763 0.00702
AFIX 43
H6A 2 0.739046 0.459054 0.035809 11.00000 -1.20000
AFIX 0
C7 1 0.698915 0.549474 0.136037 11.00000 0.01804 0.06310 =
0.02998 0.00892 0.00253 -0.00228
AFIX 43
H7A 2 0.758369 0.590810 0.164911 11.00000 -1.20000
AFIX 0
C8 1 0.626439 0.566909 0.168229 11.00000 0.01969 0.04096 =
0.01828 0.01014 0.00672 -0.00076
AFIX 43
H8A 2 0.634920 0.621992 0.219118 11.00000 -1.20000
AFIX 0
C9 1 0.537167 0.503746 0.126899 11.00000 0.01926 0.02475 =
0.01684 0.00986 0.00097 0.00449
C10 1 0.457862 0.518468 0.159330 11.00000 0.01694 0.01952 =
0.01315 0.00327 0.00045 0.00000
C11 1 0.471103 0.609447 0.238831 11.00000 0.01247 0.02567 =
0.01546 0.00069 -0.00025 0.00098
C12 1 0.448727 0.773654 0.238250 11.00000 0.01960 0.02706 =
0.01949 0.00043 0.00298 -0.00662
AFIX 43
H12A 2 0.418601 0.824942 0.187710 11.00000 -1.20000
AFIX 0
C13 1 0.469042 0.868665 0.310311 11.00000 0.02597 0.02907 =
0.03793 -0.00708 0.00857 -0.00051
AFIX 43
H13A 2 0.452796 0.982392 0.308466 11.00000 -1.20000
AFIX 0
C14 1 0.512774 0.794398 0.383458 11.00000 0.02990 0.03189 =
0.01589 -0.01076 0.00634 -0.00584
AFIX 43
H14A 2 0.528695 0.858701 0.432056 11.00000 -1.20000
AFIX 0
C15 1 0.533934 0.627886 0.387443 11.00000 0.01575 0.03867 =
0.01528 -0.00529 0.00532 -0.01150
C16 1 0.580038 0.548709 0.463387 11.00000 0.01556 0.05115 =
0.01757 -0.00044 0.00113 -0.00635
AFIX 43
H16A 2 0.598484 0.611941 0.512237 11.00000 -1.20000
AFIX 0
C17 1 0.597672 0.379947 0.465495 11.00000 0.01563 0.05465 =
0.01762 0.01153 0.00408 0.00066
AFIX 43
H17A 2 0.627933 0.328737 0.516022 11.00000 -1.20000
AFIX 0
C18 1 0.572024 0.286071 0.395658 11.00000 0.02210 0.03515 =
0.02811 0.01226 0.00485 0.00177
AFIX 43
H18A 2 0.582793 0.170248 0.398670 11.00000 -1.20000
AFIX 0
C19 1 0.530904 0.358254 0.321436 11.00000 0.01861 0.03560 =
0.01810 0.00614 0.00462 -0.00296
AFIX 43
H19A 2 0.515217 0.292058 0.273464 11.00000 -1.20000
AFIX 0
C20 1 0.511715 0.528472 0.315431 11.00000 0.01085 0.02427 =
0.01090 0.00106 -0.00174 -0.00301
C21 1 0.133054 0.354242 0.375481 11.00000 0.02823 0.02098 =
0.01640 -0.00294 0.00364 -0.00296
C22 1 0.145525 0.231650 0.438783 11.00000 0.02290 0.03289 =
0.02449 0.01042 0.00450 0.01068
AFIX 43
H22A 2 0.205899 0.187566 0.462407 11.00000 -1.20000
AFIX 0
C23 1 0.072386 0.177775 0.465393 11.00000 0.02796 0.04858 =
0.02316 0.01697 0.01171 0.00411
AFIX 43
H23A 2 0.082741 0.097352 0.507647 11.00000 -1.20000
AFIX 0
C24 1 -0.017817 0.238230 0.431883 11.00000 0.02604 0.03724 =
0.02613 0.01243 0.01046 -0.00210
C25 1 -0.094831 0.185630 0.458195 11.00000 0.02873 0.06958 =
0.03950 0.02009 0.01410 -0.00443
AFIX 43
H25A 2 -0.086796 0.101458 0.498497 11.00000 -1.20000
AFIX 0
C26 1 -0.181126 0.253450 0.426819 11.00000 0.02752 0.07985 =
0.04667 0.01469 0.01743 -0.00458
AFIX 43
H26A 2 -0.231931 0.216693 0.446126 11.00000 -1.20000
AFIX 0
C27 1 -0.195582 0.375043 0.367255 11.00000 0.01832 0.06314 =
0.03495 0.00834 0.00664 0.00507
AFIX 43
H27A 2 -0.256108 0.420341 0.345894 11.00000 -1.20000
AFIX 0
C28 1 -0.123882 0.429625 0.339342 11.00000 0.02032 0.04791 =
0.02117 0.00834 -0.00294 0.00927
AFIX 43
H28A 2 -0.135154 0.512162 0.298050 11.00000 -1.20000
AFIX 0
C29 1 -0.032773 0.366692 0.370196 11.00000 0.01991 0.03118 =
0.01669 0.00017 0.00325 0.00047
C30 1 0.044757 0.419628 0.341548 11.00000 0.02453 0.02080 =
0.01062 -0.00074 0.00290 0.00164
C31 1 0.028317 0.549683 0.276835 11.00000 0.01409 0.03117 =
0.01740 0.00148 0.00382 0.00127
C32 1 0.037166 0.713173 0.297303 11.00000 0.02962 0.02703 =
0.02428 -0.00438 0.00251 0.00104
AFIX 43
H32A 2 0.060238 0.744212 0.353073 11.00000 -1.20000
AFIX 0
C33 1 0.012379 0.836904 0.236434 11.00000 0.03735 0.02518 =
0.04859 0.00099 0.00901 0.00794
AFIX 43
H33A 2 0.020383 0.950138 0.251441 11.00000 -1.20000
AFIX 0
C34 1 -0.022759 0.794633 0.156751 11.00000 0.03263 0.02476 =
0.03741 0.01722 0.00623 0.00784
AFIX 43
H34A 2 -0.039996 0.879465 0.116849 11.00000 -1.20000
AFIX 0
C35 1 -0.034267 0.629878 0.131815 11.00000 0.01398 0.02860 =
0.02901 0.01178 0.00428 0.00496
C36 1 -0.070768 0.580345 0.049390 11.00000 0.01186 0.05392 =
0.02085 0.02117 -0.00178 0.00587
AFIX 43
H36A 2 -0.091682 0.662688 0.008697 11.00000 -1.20000
AFIX 0
C37 1 -0.076822 0.420010 0.026745 11.00000 0.02401 0.05579 =
0.01983 0.00204 0.00259 -0.00491
AFIX 43
H37A 2 -0.101119 0.391209 -0.029205 11.00000 -1.20000
AFIX 0
C38 1 -0.046877 0.293978 0.086521 11.00000 0.02956 0.04978 =
0.02494 -0.00954 0.00434 -0.01494
AFIX 43
H38A 2 -0.050523 0.181304 0.070265 11.00000 -1.20000
AFIX 0
C39 1 -0.012777 0.334622 0.167504 11.00000 0.02377 0.03176 =
0.01954 0.00381 0.00227 0.00142
AFIX 43
H39A 2 0.006246 0.249799 0.207183 11.00000 -1.20000
AFIX 0
C40 1 -0.005807 0.500747 0.192131 11.00000 0.01434 0.02502 =
0.01874 -0.00041 0.00127 -0.00203
C41 1 0.175287 0.534089 0.079251 11.00000 0.01999 0.03036 =
0.02111 0.00589 0.00103 0.00201
AFIX 23
H41A 2 0.185817 0.559147 0.025372 11.00000 -1.20000
H41B 2 0.113093 0.487100 0.076259 11.00000 -1.20000
AFIX 0
C42 1 0.216433 0.654830 0.149366 11.00000 0.02317 0.02131 =
0.03116 0.01077 0.00174 0.00804
AFIX 23
H42A 2 0.178718 0.678782 0.187921 11.00000 -1.20000
H42B 2 0.251491 0.750877 0.137000 11.00000 -1.20000
AFIX 0
C43 1 0.272341 0.603927 0.366640 11.00000 0.02775 0.02543 =
0.02051 -0.00420 0.00636 -0.00803
AFIX 23
H43A 2 0.307733 0.659909 0.332661 11.00000 -1.20000
H43B 2 0.230585 0.677667 0.387094 11.00000 -1.20000
AFIX 0
C44 1 0.322202 0.466706 0.423819 11.00000 0.02135 0.02979 =
0.01303 -0.00229 -0.00369 -0.00456
AFIX 23
H44A 2 0.310089 0.459130 0.478239 11.00000 -1.20000
H44B 2 0.387221 0.441375 0.423817 11.00000 -1.20000
AFIX 0
CL3 4 0.793985 0.017868 0.177532 10.75000 0.07258 0.09652 =
0.13299 -0.00944 0.04442 -0.00689
CL4 4 0.627306 0.017196 0.225405 10.75000 0.11942 0.07886 =
0.18344 -0.04475 0.10004 -0.02139
C45 1 0.694349 0.101658 0.179367 10.75000 0.06758 0.06586 =
0.06305 -0.00881 0.00029 -0.00133
AFIX 23
H45A 2 0.708538 0.213615 0.202934 10.75000 -1.20000
H45B 2 0.657886 0.116716 0.121765 10.75000 -1.20000
SADI CL3 C45 CL4 C45
DELU CL3 CL4 C45
SIMU CL3 CL4 C45

HKLF 4

REM ljh48 in P2(1)
REM R1 = 0.0325 for 5534 Fo > 4sig(Fo) and 0.0358 for all 6013 data
REM 469 parameters refined using 17 restraints

END

WGHT 0.0573 0.0000
REM Highest difference peak 2.000, deepest hole -0.870, 1-sigma level 0.133
Q1 1 0.7454 -0.1333 0.3332 11.00000 0.05 2.00
Q2 1 0.2591 0.1224 0.2378 11.00000 0.05 1.98
Q3 1 0.2592 0.3731 0.2389 11.00000 0.05 1.92
Q4 1 0.2063 0.2454 0.2622 11.00000 0.05 1.80
Q5 1 0.3147 0.2436 0.2155 11.00000 0.05 1.49
;