An unusual alkylidyne homologation.
Han, Yong-Shen; Hill, Anthony F.; Kong, Richard Y.; Chemical communications (Cambridge, England) 54 (2018) 2292–2295; doi:10.1039/c8cc00119g

data_7121254
_publ_section_title
;
 An unusual alkylidyne homologation.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2292
_journal_page_last               2295
_journal_paper_doi               10.1039/c8cc00119g
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C32 H59 Cl3 P2 W'
_chemical_formula_sum            'C32 H59 Cl3 P2 W'
_chemical_formula_weight         795.93
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-11-24 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.7156(4)
_cell_length_b                   23.4584(6)
_cell_length_c                   23.8845(7)
_cell_measurement_reflns_used    10945
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.7440
_cell_measurement_theta_min      3.6890
_cell_volume                     8245.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -103.00  -9.00   1.00   22.50    --  -36.03 -77.00-120.00   94
  2  \w    -65.00  32.00   1.00   22.50    --  -36.03  19.00 120.00   97
  3  \w   -105.00  -7.00   1.00   22.50    --  -36.03 -19.00  90.00   98
  4  \w      1.00  75.00   1.00   22.50    --   36.03 -99.00   0.00   74
  5  \w     32.00  88.00   1.00   22.50    --   36.03-125.00-180.00   56
  6  \w     39.00 125.00   1.00   87.50    --  107.33 -45.00-120.00   86
  7  \w     39.00 121.00   1.00   87.50    --  107.33 -45.00 -30.00   82
  8  \w     37.00 115.00   1.00   87.50    --  107.33-111.00 120.00   78
  9  \w     91.00 156.00   1.00   87.50    --  107.33  45.00-150.00   65
 10  \w     39.00 124.00   1.00   87.50    --  107.33 -45.00  60.00   85
 11  \w     98.00 172.00   1.00   87.50    --  107.33  77.00  30.00   74
 12  \w     59.00 134.00   1.00   87.50    --  107.33 -77.00 120.00   75
 13  \w     54.00 110.00   1.00   87.50    --  107.33-111.00 -60.00   56
 14  \w     48.00 109.00   1.00   87.50    --  107.33 -95.00   0.00   61
 15  \w     50.00 164.00   1.00   87.50    --  107.33   0.00-180.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0384072000
_diffrn_orient_matrix_UB_12      0.0476325000
_diffrn_orient_matrix_UB_13      0.0376008000
_diffrn_orient_matrix_UB_21      0.0921366000
_diffrn_orient_matrix_UB_22      -0.0043050000
_diffrn_orient_matrix_UB_23      -0.0303511000
_diffrn_orient_matrix_UB_31      -0.0317240000
_diffrn_orient_matrix_UB_32      0.0450067000
_diffrn_orient_matrix_UB_33      -0.0426737000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            44726
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.032
_diffrn_reflns_theta_min         3.701
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.830
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       block
_exptl_crystal_F_000             3248
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.031
_refine_diff_density_max         2.563
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         8039
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+31.5706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5937
_reflns_number_total             8039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00119g2.cif
_cod_data_source_block           rk14_scaled
_cod_depositor_comments
'Adding full bibliography for 7121252--7121255.cif.'
_cod_database_code               7121254
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         C33H58Cl4O2P2SiW
_chemical_oxdiff_usercomment     'small triangular plate'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C124) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C108) \\sim Ueq, Uanis(C107) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C27) = Uanis(C31) = Uanis(C30) = Uanis(C29) = Uanis(C32)
Uanis(C129) = Uanis(C130) = Uanis(C132) = Uanis(C131) = Uanis(C127)
Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C15) = Uanis(C16) = Uanis(C17)
Uanis(C115) = Uanis(C116) = Uanis(C117) = Uanis(C118) = Uanis(C119) =
Uanis(C120)
Uanis(C121) = Uanis(C126) = Uanis(C125) = Uanis(C3BA) = Uanis(C123) =
Uanis(C122)
Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C3BA) = Uanis(C26)
3. Others
 Sof(C127)=Sof(H127)=Sof(C129)=Sof(H12C)=Sof(H12D)=Sof(C130)=Sof(H13C)=
 Sof(H13D)=Sof(C131)=Sof(H13E)=Sof(H13F)=Sof(C132)=Sof(H13G)=Sof(H13H)=
 Sof(H28C)=Sof(H28D)=1-FVAR(1)
 Sof(C27)=Sof(H27)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C30)=Sof(H30A)=Sof(H30B)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H28A)=Sof(H28B)=
 FVAR(1)
 Sof(C15)=Sof(H15)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C16)=Sof(H16A)=
 Sof(H16B)=1-FVAR(2)
 Sof(C115)=Sof(H115)=Sof(C117)=Sof(H11C)=Sof(H11D)=Sof(C120)=Sof(H12E)=
 Sof(H12F)=Sof(C116)=Sof(H11E)=Sof(H11F)=Sof(C119)=Sof(H11G)=Sof(H11H)=
 Sof(C118)=Sof(H11I)=Sof(H11J)=FVAR(2)
 Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(C124)=Sof(H12O)=Sof(H12P)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C23)=Sof(H23A)=
 Sof(H23B)=1-FVAR(3)
 Sof(C121)=Sof(H121)=Sof(C122)=Sof(H12G)=Sof(H12H)=Sof(C3BA)=Sof(H3BA)=
 Sof(H3BB)=Sof(C126)=Sof(H12I)=Sof(H12J)=Sof(C123)=Sof(H12K)=Sof(H12L)=
 Sof(C125)=Sof(H12M)=Sof(H12N)=FVAR(3)
 Sof(C107)=Sof(H10C)=Sof(H10D)=Sof(C108)=Sof(H10E)=Sof(H10F)=1-FVAR(4)
 Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C7)=Sof(H7A)=Sof(H7B)=FVAR(4)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C27(H27), C127(H127), C115(H115), C15(H15), C121(H121), C21(H21)
4.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C10(H10A,H10B), C2(H2A,H2B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C8(H8A,H8B), C7(H7A,H7B), C31(H31A,H31B), C30(H30A,H30B),
 C29(H29A,H29B), C32(H32A,H32B), C129(H12C,H12D), C130(H13C,H13D), C131(H13E,
 H13F), C132(H13G,H13H), C117(H11C,H11D), C120(H12E,H12F), C116(H11E,H11F),
 C119(H11G,H11H), C118(H11I,H11J), C20(H20A,H20B), C19(H19A,H19B), C18(H18A,
 H18B), C17(H17A,H17B), C16(H16A,H16B), C122(H12G,H12H), C3BA(H3BA,H3BB),
 C126(H12I,H12J), C123(H12K,H12L), C125(H12M,H12N), C22(H22A,H22B), C26(H26A,
 H26B), C124(H12O,H12P), C24(H24A,H24B), C23(H23A,H23B), C28(H28A,H28B),
 C28(H28C,H28D), C107(H10C,H10D), C108(H10E,H10F)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_fab_checksum              39966
_ins_header
;
TITL RK14_scaled in Pbca 
REM Pbca (#61 in standard setting)
CELL 1.54184  14.715593  23.458353  23.884463  90.0000  90.0000  90.0000
ZERR   11.00   0.000352   0.000593   0.000712   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H O Si P Cl W
UNIT 363.00 638.00 22.00 11.00 22.00 44.00 11.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.353
_oxdiff_exptl_absorpt_empirical_full_min 0.771