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_7121252
_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         'C33 H58.7 Cl3.3 O2 P2 Si W, C H Cl3'
_chemical_formula_sum            'C34 H59.7 Cl6.3 O2 P2 Si W'
_chemical_formula_weight         997.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-11-24 deposited with the CCDC.
2018-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.632(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9285(2)
_cell_length_b                   19.4442(4)
_cell_length_c                   20.0693(5)
_cell_measurement_reflns_used    16746
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      71.7070
_cell_measurement_theta_min      4.0750
_cell_volume                     4216.34(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
;
_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    'ShelXT (Sheldrick, 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 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega   23.00   90.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       36.1504 -125.0000 -120.0000 67

  2 omega   23.00   90.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       36.1504 -125.0000 -180.0000 67

  3 omega    9.00  104.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       36.1504   77.0000   30.0000 95

  4 omega  -31.00   63.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       36.1504  -77.0000  -90.0000 94

  5 omega  -33.00  105.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       36.1504    0.0000 -120.0000 138

  6 omega   37.00   91.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077  -30.0000   30.0000 54

  7 omega   37.00  115.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077 -111.0000  -90.0000 78

  8 omega   89.00  175.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077   45.0000   60.0000 86

  9 omega   37.00   91.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077  -30.0000 -120.0000 54

 10 omega   68.00  177.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077   15.0000 -180.0000 109

 11 omega   37.00  109.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077  -95.0000   30.0000 72

 12 omega   37.00   91.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077  -30.0000   90.0000 54

 13 omega   37.00   91.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077  -30.0000  150.0000 54

 14 omega   37.00  109.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077  -95.0000  -60.0000 72

 15 omega   38.00   98.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077  -45.0000  -60.0000 60

 16 omega   38.00   98.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077  -45.0000    0.0000 60

 17 omega   39.00  133.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077  -77.0000   90.0000 94

 18 omega   17.00  105.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       36.1504   38.0000    0.0000 88

 19 omega    1.00   75.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       36.1504  -99.0000   60.0000 74

 20 omega   17.00  105.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       36.1504   38.0000  -60.0000 88

 21 omega    9.00  104.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       36.1504   77.0000 -180.0000 95

 22 omega    1.00   28.00   1.0000    3.5300
omega____ theta____ kappa____ phi______ frames
    -       36.1504   92.0000   78.3722 27

 23 omega   89.00  175.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077   45.0000    0.0000 86

 24 omega   68.00  177.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077   15.0000  -60.0000 109

 25 omega   80.00  174.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077   77.0000  -60.0000 94

 26 omega   89.00  175.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077   45.0000   90.0000 86

 27 omega   89.00  175.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077   45.0000   30.0000 86

 28 omega   89.00  175.00   1.0000   14.1300
omega____ theta____ kappa____ phi______ frames
    -      106.7077   45.0000 -150.0000 86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_UB_11      -0.1327275000
_diffrn_orient_matrix_UB_12      -0.0267576000
_diffrn_orient_matrix_UB_13      -0.0002071000
_diffrn_orient_matrix_UB_21      0.0314398000
_diffrn_orient_matrix_UB_22      -0.0652193000
_diffrn_orient_matrix_UB_23      -0.0376226000
_diffrn_orient_matrix_UB_31      0.0413028000
_diffrn_orient_matrix_UB_32      -0.0362469000
_diffrn_orient_matrix_UB_33      0.0679015000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44515
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.801
_diffrn_reflns_theta_min         3.182
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.966
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58403
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       plate
_exptl_crystal_F_000             2019
_exptl_crystal_size_max          0.1039
_exptl_crystal_size_mid          0.0551
_exptl_crystal_size_min          0.0188
_refine_diff_density_max         2.616
_refine_diff_density_min         -1.624
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0460P)^2^+10.4195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0973
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6702
_reflns_number_total             8184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00119g2.cif
_cod_data_source_block           Compound_3_scaled
_cod_depositor_comments
'Adding full bibliography for 7121252--7121255.cif.'
_cod_original_cell_volume        4216.35(17)
_cod_original_formula_sum        'C34 H59.70 Cl6.30 O2 P2 Si W'
_cod_database_code               7121252
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl2(0.7) Cl3(0.6) H1A(0.4) H1B(0.3)
 Fixed Uiso: H1A(0.048) H1B(0.048)
 Fixed X: H1A(0.704) H1B(0.7034)
 Fixed Y: H1A(0.7022) H1B(0.7946)
 Fixed Z: H1A(0.3945) H1B(0.3968)
3.a Ternary CH refined with riding coordinates:
 C11(H11), C21(H21), C31(H31), C41(H41), C51(H51)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
  C25(H25A,H25B), C26(H26A,H26B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,
 H34B), C35(H35A,H35B), C36(H36A,H36B), C42(H42A,H42B), C43(H43A,H43B),
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              96539
_ins_header
;
TITL yhc012_scaled in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184  10.928546  19.444180  20.069315  90.0000  98.6322  90.0000
ZERR    6.00   0.000233   0.000405   0.000525   0.0000   0.0023   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H O Si P Br W
UNIT 192.00 342.00 12.00 6.00 12.00 6.00 6.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'