A [C<sub>1</sub> + C<sub>2</sub>] route to propargylidyne complexes.
Hill, Anthony F.; Manzano, Richard A.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6596–6610; doi:10.1039/c9dt00876d

data_7701669
_publ_section_title
;
 A [C<sub>1</sub> + C<sub>2</sub>] route to propargylidyne complexes.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6596
_journal_page_last               6610
_journal_paper_doi               10.1039/c9dt00876d
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C39 H37 B N6 O2 W, C H2 Cl2'
_chemical_formula_sum            'C40 H39 B Cl2 N6 O2 W'
_chemical_formula_weight         901.33
_chemical_name_systematic        W(CCCCPh3)(CO)2Tp*
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-11
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-15 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.8000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0666(2)
_cell_length_b                   12.8247(2)
_cell_length_c                   34.3229(5)
_cell_measurement_reflns_used    15259
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.6500
_cell_measurement_theta_min      4.6250
_cell_volume                     8114.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(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    -21.00  54.00   1.00   10.00    --   36.95 -38.00 150.00   75
  2  \w     48.00  89.00   1.00   10.00    --   36.95  57.00  90.00   41
  3  \w     74.00 100.00   1.00   10.00    --   36.95  57.00  30.00   26
  4  \w     20.00  97.00   1.00   10.00    --   36.95  57.00 150.00   77
  5  \w     20.00  59.00   1.00   10.00    --   36.95  57.00  30.00   39
  6  \w     56.00  88.00   1.00   10.00    --   36.95-125.00 -90.00   32
  7  \w     24.00  97.00   1.00   10.00    --   36.95  38.00 -30.00   73
  8  \w     64.00  96.00   1.00   10.00    --   36.95  19.00 -90.00   32
  9  \w     42.00 115.00   1.00   40.00    --  111.00-111.00-150.00   73
 10  \w     89.00 114.00   1.00   40.00    --  111.00-111.00 150.00   25
 11  \w     69.00 178.00   1.00   40.00    --  111.00  12.00-180.00  109
 12  \w    104.00 141.00   1.00   40.00    --  111.00  64.00  60.00   37
 13  \w     78.00 104.00   1.00   40.00    --  111.00 -19.00 125.43   26
 14  \w    111.00 176.00   1.00   40.00    --  111.00  64.00 150.00   65
 15  \w     96.00 122.00   1.00   40.00    --  111.00 -50.00  90.00   26
 16  \w     85.00 116.00   1.00   40.00    --  111.00 -38.00  30.00   31
 17  \w     43.00  71.00   1.00   40.00    --  111.00 -38.00  30.00   28
 18  \w    136.00 172.00   1.00   40.00    --  111.00 111.00-180.00   36
 19  \w     94.00 178.00   1.00   40.00    --  111.00  64.00  90.00   84
 20  \w    131.00 175.00   1.00   40.00    --  111.00  38.00-150.00   44
 21  \w     63.00 104.00   1.00   40.00    --  111.00-111.00 -90.00   41
 22  \w     49.00  74.00   1.00   40.00    --  111.00 -77.00 -30.00   25
 23  \w    106.00 136.00   1.00   40.00    --  111.00 -77.00 -30.00   30
 24  \w     99.00 130.00   1.00   40.00    --  111.00 -64.00 120.00   31
 25  \w     83.00 127.00   1.00   40.00    --  111.00 -64.00-180.00   44
 26  \w     62.00 104.00   1.00   40.00    --  111.00 -64.00  90.00   42
 27  \w    120.00 177.00   1.00   40.00    --  111.00 111.00  60.00   57
 28  \w     78.00 117.00   1.00   40.00    --  111.00 -92.00 -90.00   39
 29  \w     51.00 110.00   1.00   40.00    --  111.00-111.00  60.00   59
;
_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      0.0718864000
_diffrn_orient_matrix_UB_12      0.0207748000
_diffrn_orient_matrix_UB_13      0.0317597000
_diffrn_orient_matrix_UB_21      0.0426172000
_diffrn_orient_matrix_UB_22      -0.0389248000
_diffrn_orient_matrix_UB_23      -0.0297123000
_diffrn_orient_matrix_UB_31      0.0014498000
_diffrn_orient_matrix_UB_32      0.1116491000
_diffrn_orient_matrix_UB_33      -0.0163282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            26020
_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         73.713
_diffrn_reflns_theta_min         3.695
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.812
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             3600
_exptl_crystal_recrystallization_method
'Crystals were grown from vapour-vapour diffusion of heptane into a dichloromethane solution.'
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.973
_refine_diff_density_min         -1.567
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8115
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+21.7003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7353
_reflns_number_total             8115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00876d1.cif
_cod_data_source_block           wccccph3scale
_cod_database_code               7701669
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C39 H36 B1 N6 O2 W1'
_chemical_oxdiff_usercomment
'Crystal grown from v/v diffusion of heptane into DCM'
_reflns_odcompleteness_completeness 97.81
_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,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2-C101 = Cl10-C101
 1.7 with sigma of 0.01
3. Others
 Sof(H10c)=Sof(H10d)=Sof(Cl2)=1-FVAR(1)
 Sof(Cl10)=Sof(H10a)=Sof(H10b)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C101(H10a,H10b), C101(H10c,H10d)
4.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C24(H18), C32(H31), C23(H17), C14(H12), C20(H14), C22(H16), C18(H8),
  C21(H15), C8(H20), C17(H9), C16(H10), C29(H36), C15(H11), C9(H21), C12(H24),
 C10(H22), C11(H23)
4.c Idealised Me refined as rotating group:
 C35(H29a,H29b,H29c), C34(H28a,H28b,H28c), C39(H34a,H34b,H34c), C37(H39a,H39b,
 H39c), C36(H38a,H38b,H38c), C38(H33a,H33b,H33c)
;
_shelx_res_checksum              85969
_shelx_fab_checksum              59680
_ins_header
'TITL WCCCCPh3scale in Ia REM Ia (#9 in standard setting) CELL 1.54184 19.066561 12.824714 34.322878 90.0000 104.7999 90.0000 ZERR 8.00 0.000245 0.000153 0.000484 0.0000 0.0014 0.0000 LATT -2 SYMM x+1/2,-y, z SFAC C H B N O W UNIT 312.00 288.00 8.00 48.00 16.00 8.00 TREF HKLF 4 END'
_olex2_submission_original_sample_id WCCCCPh3
_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 1.310
_oxdiff_exptl_absorpt_empirical_full_min 0.809