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_7701671
_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         'C52 H54 Au2 B2 Cl2 N12 O4 Si W2, C H Cl3'
_chemical_formula_sum            'C53 H55 Au2 B2 Cl5 N12 O4 Si W2'
_chemical_formula_weight         1912.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-18
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-18 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                100.499(2)
_cell_angle_beta                 111.095(2)
_cell_angle_gamma                99.537(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7417(2)
_cell_length_b                   15.7262(3)
_cell_length_c                   17.5006(3)
_cell_measurement_reflns_used    17573
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5140
_cell_measurement_theta_min      2.7800
_cell_volume                     3113.06(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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 1.000
_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     19.00  55.00   1.00    3.73    --   37.04 -38.00   0.00   36
  2  \w     22.00  54.00   1.00    3.73    --   37.04 -57.00   0.00   32
  3  \w     30.00  74.00   1.00    3.73    --   37.04 -99.00 -30.00   44
  4  \w     61.00  89.00   1.00    3.73    --   37.04-125.00 -90.00   28
  5  \w     34.00  74.00   1.00    3.73    --   37.04-125.00 -30.00   40
  6  \w     23.00  50.00   1.00    3.73    --   37.04 -77.00  90.00   27
  7  \w     39.00  90.00   1.00    3.73    --   37.04-125.00 120.00   51
  8  \w     88.00 116.00   1.00   14.89    --  111.00-111.00 150.00   28
  9  \w     80.00 135.00   1.00   14.89    --  111.00 -92.00 150.00   55
 10  \w     78.00 111.00   1.00   14.89    --  111.00-111.00  30.00   33
 11  \w     93.00 132.00   1.00   14.89    --  111.00 -77.00  30.00   39
 12  \w    101.00 126.00   1.00   14.89    --  111.00 -50.00 -30.00   25
 13  \w    102.00 136.00   1.00   14.89    --  111.00 -25.00 -90.00   34
 14  \w    127.00 156.00   1.00   14.89    --  111.00 -12.00-120.00   29
 15  \w    127.00 154.00   1.00   14.89    --  111.00   0.00-150.00   27
 16  \w    117.00 144.00   1.00   14.89    --  111.00  50.00-120.00   27
 17  \w    123.00 150.00   1.00   14.89    --  111.00  64.00 -90.00   27
 18  \w    140.00 165.00   1.00   14.89    --  111.00 111.00 -60.00   25
 19  \w    103.00 130.00   1.00   14.89    --  111.00 111.00   0.00   27
 20  \w    144.00 177.00   1.00   14.89    --  111.00  55.00  85.00   33
 21  \w    149.00 174.00   1.00   14.89    --  111.00  25.00 150.00   25
 22  \w    121.00 148.00   1.00   14.89    --  111.00  12.00  90.00   27
 23  \w    111.00 136.00   1.00   14.89    --  111.00  55.00  85.00   25
 24  \w     92.00 141.00   1.00   14.89    --  111.00  25.00 150.00   49
 25  \w     76.00 124.00   1.00   14.89    --  111.00 -64.00  30.00   48
 26  \w     93.00 138.00   1.00   14.89    --  111.00 -92.00 -60.00   45
 27  \w    100.00 134.00   1.00   14.89    --  111.00 -25.00-150.00   34
 28  \w    113.00 146.00   1.00   14.89    --  111.00 -12.00-180.00   33
 29  \w    103.00 128.00   1.00   14.89    --  111.00 -50.00-180.00   25
 30  \w     96.00 123.00   1.00   14.89    --  111.00 -12.00-120.00   27
 31  \w     88.00 136.00   1.00   14.89    --  111.00  25.00-150.00   48
 32  \w     97.00 178.00   1.00   14.89    --  111.00  50.00-150.00   81
 33  \w     97.00 122.00   1.00   14.89    --  111.00  50.00 -60.00   25
 34  \w     95.00 127.00   1.00   14.89    --  111.00  50.00 -90.00   32
 35  \w     89.00 157.00   1.00   14.89    --  111.00  25.00-180.00   68
 36  \w     90.00 130.00   1.00   14.89    --  111.00 -64.00-180.00   40
 37  \w     82.00 116.00   1.00   14.89    --  111.00-111.00-120.00   34
 38  \w     70.00 105.00   1.00   14.89    --  111.00 -64.00 -60.00   35
 39  \w     66.00 116.00   1.00   14.89    --  111.00-111.00 -30.00   50
 40  \w     78.00 110.00   1.00   14.89    --  111.00-111.00  60.00   32
 41  \w     67.00  92.00   1.00   14.89    --  111.00 -92.00 120.00   25
 42  \w     64.00 124.00   1.00   14.89    --  111.00 -64.00 150.00   60
 43  \w     58.00  98.00   1.00   14.89    --  111.00 -77.00 150.00   40
 44  \w     58.00 103.00   1.00   14.89    --  111.00-111.00 120.00   45
 45  \w     57.00 103.00   1.00   14.89    --  111.00 -77.00 107.29   46
 46  \w     59.00  92.00   1.00   14.89    --  111.00 -25.00 150.00   33
 47  \w     46.00  77.00   1.00   14.89    --  111.00 -50.00 150.00   31
 48  \w     44.00  79.00   1.00   14.89    --  111.00 -50.00 120.00   35
 49  \w     42.00  75.00   1.00   14.89    --  111.00 -92.00 150.00   33
 50  \w     43.00  98.00   1.00   14.89    --  111.00-111.00  90.00   55
 51  \w     44.00  71.00   1.00   14.89    --  111.00-111.00 150.00   27
 52  \w     46.00 102.00   1.00   14.89    --  111.00 -38.00  30.00   56
 53  \w     62.00  98.00   1.00   14.89    --  111.00 -77.00 -60.00   36
 54  \w     66.00  92.00   1.00   14.89    --  111.00 -25.00 -90.00   26
 55  \w     73.00 100.00   1.00   14.89    --  111.00   0.00-150.00   27
 56  \w     57.00 100.00   1.00   14.89    --  111.00 -55.00 -57.00   43
 57  \w     46.00 126.00   1.00   14.89    --  111.00 -38.00 -90.00   80
 58  \w     50.00 101.00   1.00   14.89    --  111.00-111.00 -60.00   51
 59  \w     45.00  72.00   1.00   14.89    --  111.00 -92.00 -60.00   27
 60  \w     43.00  74.00   1.00   14.89    --  111.00 -50.00 -90.00   31
 61  \w     41.00  89.00   1.00   14.89    --  111.00 -12.00-180.00   48
 62  \w     45.00 103.00   1.00    3.73    --   37.04  57.00-180.00   58
 63  \w     14.00  98.00   1.00    3.73    --   37.04  77.00   0.00   84
 64  \w     44.00  99.00   1.00    3.73    --   37.04  57.00 150.00   55
 65  \w      2.00  27.00   1.00    3.73    --   37.04 -99.00 -30.00   25
 66  \w      1.00  50.00   1.00    3.73    --   37.04 -99.00-120.00   49
 67  \w    -15.00  28.00   1.00    3.73    --   37.04 -57.00-120.00   43
 68  \w    -30.00  12.00   1.00    3.73    --   37.04 -57.00   0.00   42
 69  \w    -29.00  -4.00   1.00    3.73    --   37.04 -57.00 -30.00   25
 70  \w    -26.00  66.00   1.00    3.73    --   37.04 -19.00   0.00   92
 71  \w     41.00  68.00   1.00   14.89    --  111.00 -25.00 120.00   27
 72  \w    -21.00  40.00   1.00    3.73    --   37.04 -38.00 -90.00   61
 73  \w    107.00 132.00   1.00   14.89    --  111.00 178.00 -90.00   25
 74  \w     97.00 122.00   1.00   14.89    --  111.00 178.00 -30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0286856000
_diffrn_orient_matrix_UB_12      -0.0636413000
_diffrn_orient_matrix_UB_13      -0.0633616000
_diffrn_orient_matrix_UB_21      0.0677754000
_diffrn_orient_matrix_UB_22      0.0809122000
_diffrn_orient_matrix_UB_23      -0.0156603000
_diffrn_orient_matrix_UB_31      0.1118807000
_diffrn_orient_matrix_UB_32      -0.0016318000
_diffrn_orient_matrix_UB_33      0.0728226000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40111
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.590
_diffrn_reflns_theta_max         66.590
_diffrn_reflns_theta_min         3.498
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.908
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    2.040
_exptl_crystal_description       needle
_exptl_crystal_F_000             1808
_exptl_crystal_recrystallization_method
'Crystals were grown from vapour-vapour diffusion of hexane in to a chloroform solution.'
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.042
_refine_diff_density_max         7.529
_refine_diff_density_min         -5.307
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         10989
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0644
_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^)+(0.1087P)^2^+66.5357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1813
_refine_ls_wR_factor_ref         0.1893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9706
_reflns_number_total             10989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00876d1.cif
_cod_data_source_block           ram-138scaleabscorrect3
_cod_original_cell_volume        3113.06(10)
_cod_database_code               7701671
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C63 H65 Au2 B2 Cl5 N12 O4 Si1 W2'
_chemical_oxdiff_usercomment
'Brown needles grown from chloroform/pentane vdiffusion'
_reflns_odcompleteness_completeness 98.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2), C101(H101)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C29(H29), C34(H34), C39(H39), C44(H44),
  C49(H49)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C42(H42A,
 H42B,H42C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C51(H51A,H51B,H51C),
 C52(H52A,H52B,H52C)
;
_shelx_res_checksum              55650
_shelx_fab_checksum              56925
_ins_header
;
TITL RAM-138scaleabscorrect3 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  12.741684  15.726221  17.500558 100.4994 111.0946  99.5366
ZERR    2.00   0.000222   0.000343   0.000289   0.0016   0.0016   0.0016
LATT  1
SFAC C H B N O Si Cl W Au
UNIT 126.00 130.00 4.00 24.00 8.00 2.00 10.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id W2Au2{CCC(SiPh2)(CCC}(CO)4Cl(Tp*)2
_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 2.255
_oxdiff_exptl_absorpt_empirical_full_min 0.592