An anionic nucleophilic d(4) carbyne complex.
Hill, Anthony F.; Kong, Richard Y.; Chemical communications (Cambridge, England) 53 (2017) 2032–2035; doi:10.1039/c6cc09718a

data_7119545
_publ_section_title
;
 An anionic nucleophilic d(4) carbyne complex.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2032
_journal_page_last               2035
_journal_paper_doi               10.1039/c6cc09718a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C39 H62 O2 P2 Te W'
_chemical_formula_sum            'C39 H62 O2 P2 Te W'
_chemical_formula_weight         936.27
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-08 deposited with the CCDC.
2016-12-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1600(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.62715(11)
_cell_length_b                   15.6401(2)
_cell_length_c                   24.3392(3)
_cell_measurement_reflns_used    19436
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6020
_cell_measurement_theta_min      3.3500
_cell_volume                     3981.97(8)
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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   -104.00 -20.00   1.00    1.04    --  -37.20 -57.00 120.00   84
  2  \w     23.00  91.00   1.00    1.04    --   37.20-125.00 120.00   68
  3  \w    -30.00  54.00   1.00    1.04    --   37.20 -57.00 -60.00   84
  4  \w      8.00 109.00   1.00    1.04    --   37.20  19.00 -90.00  101
  5  \w    -32.00 106.00   1.00    1.04    --   37.20   0.00-120.00  138
  6  \w     23.00  91.00   1.00    1.04    --   37.20-125.00  90.00   68
  7  \w    -34.00  67.00   1.00    1.04    --   37.20 -19.00  60.00  101
  8  \w      3.00  29.00   1.00    1.04    --   37.20  91.00-179.89   26
  9  \w    100.00 178.00   1.00    4.18    --  111.00 111.00-180.00   78
 10  \w     44.00 131.00   1.00    4.18    --  111.00 -64.00 -90.00   87
 11  \w     94.00 178.00   1.00    4.18    --  111.00  50.00  90.00   84
 12  \w     42.00 146.00   1.00    4.18    --  111.00 -92.00  30.00  104
 13  \w     94.00 178.00   1.00    4.18    --  111.00  50.00 120.00   84
 14  \w     94.00 178.00   1.00    4.18    --  111.00  50.00  60.00   84
 15  \w     65.00 178.00   1.00    4.18    --  111.00  12.00  30.00  113
 16  \w     86.00 178.00   1.00    4.18    --  111.00  25.00-180.00   92
 17  \w    100.00 178.00   1.00    4.18    --  111.00 111.00 -30.00   78
 18  \w     47.00 114.00   1.00    4.18    --  111.00-111.00 -30.00   67
 19  \w     42.00 136.00   1.00    4.18    --  111.00 -25.00 150.00   94
 20  \w     47.00  74.00   1.00    4.18    --  111.00 -77.00 -90.00   27
 21  \w     85.00 123.00   1.00    4.18    --  111.00 -77.00 -90.00   38
 22  \w     95.00 122.00   1.00    4.18    --  111.00  34.00-150.77   27
 23  \w    136.00 176.00   1.00    4.18    --  111.00  34.00-150.77   40
 24  \w     44.00 126.00   1.00    4.18    --  111.00 -64.00 120.00   82
 25  \w     54.00 125.00   1.00    4.18    --  111.00 -38.00-150.00   71
 26  \w    124.00 175.00   1.00    4.18    --  111.00  25.00 150.00   51
 27  \w     87.00 112.00   1.00    4.18    --  111.00  77.00  30.00   25
 28  \w    118.00 145.00   1.00    4.18    --  111.00  31.00 107.61   27
 29  \w     68.00  95.00   1.00    4.18    --  111.00 -77.00-180.00   27
 30  \w    100.00 125.00   1.00    4.18    --  111.00 -77.00-180.00   25
 31  \w     49.00  86.00   1.00    4.18    --  111.00 -77.00 -60.00   37
 32  \w    115.00 142.00   1.00    4.18    --  111.00 111.00-150.00   27
 33  \w     43.00 115.00   1.00    4.18    --  111.00 -25.00 -60.00   72
;
_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      -0.0886764000
_diffrn_orient_matrix_UB_12      -0.0775459000
_diffrn_orient_matrix_UB_13      0.0016529000
_diffrn_orient_matrix_UB_21      0.0379222000
_diffrn_orient_matrix_UB_22      -0.0032055000
_diffrn_orient_matrix_UB_23      0.0640550000
_diffrn_orient_matrix_UB_31      -0.1113002000
_diffrn_orient_matrix_UB_32      0.0606892000
_diffrn_orient_matrix_UB_33      0.0054000000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            41443
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.984
_diffrn_reflns_theta_min         3.375
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.026
_exptl_absorpt_correction_T_max  0.33411
_exptl_absorpt_correction_T_min  0.25367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.049
_refine_diff_density_max         1.756
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         8049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+8.3595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7401
_reflns_number_total             8049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09718a2.cif
_cod_data_source_block           Compound_3c
_cod_depositor_comments
'Adding full bibliography for 7119543--7119548.cif.'
_cod_original_cell_volume        3981.98(9)
_cod_database_code               7119545
_shelxl_version_number           2013-3
_chemical_oxdiff_formula         'C39 H62 O2 P2 Te W'
_reflns_odcompleteness_completeness 98.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.a Ternary CH refined with riding coordinates:
 C16(H10), C10(H18), C22(H4), C28(H0AA)
2.b Secondary CH2 refined with riding coordinates:
 C18(H7a,H7b), C15(H9a,H9b), C21(H12a,H12b), C20(H13a,H13b), C17(H32a,H32b),
 C19(H35a,H35b), C12(H37a,H37b), C11(H42a,H42b), C13(H45a,H45b), C14(H51a,H51b),
  C27(H5a,H5b), C8(H6a,H6b), C29(H1Ab,H1Aa), C9(H11a,H11b), C33(H2Aa,H2Ab),
 C23(H16a,H16b), C30(H17a,H17b), C24(H5Aa,H5Ab), C32(H19a,H19b), C31(H20a,H20b),
  C26(H21a,H21b), C25(H22a,H22b)
2.c Aromatic/amide H refined with riding coordinates:
 C38(H25), C39(H33), C35(H44), C37(H50), C36(H61)
2.d Idealised Me refined as rotating group:
 C5(H4Aa,H4Ab,H4Ac), C3(H15a,H15b,H15c), C4(H23a,H23b,H23c)
;
_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 2.926
_oxdiff_exptl_absorpt_empirical_full_min 0.697