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_7701666
_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         'C24 H31 B N6 O2 W'
_chemical_formula_sum            'C24 H31 B N6 O2 W'
_chemical_formula_weight         630.21
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-09-05
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-14 deposited with the CCDC.	2019-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.2849(2)
_cell_length_b                   16.5974(2)
_cell_length_c                   20.0536(2)
_cell_measurement_reflns_used    36889
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.4570
_cell_measurement_theta_min      3.5460
_cell_volume                     5087.39(10)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_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    -39.00  62.00   1.00   10.00    --  -11.22  57.00  30.00  101
  2  \w    -87.00  21.00   1.00   10.00    --  -11.22 -77.00 120.00  108
  3  \w    -39.00  62.00   1.00   10.00    --  -11.22  57.00 -60.00  101
  4  \w    -83.00  17.00   1.00   10.00    --  -11.22 -57.00-120.00  100
  5  \w    -20.00  30.00   1.00   10.00    --  -11.22 -99.00 -30.00   50
  6  \w    -86.00  13.00   1.00   10.00    --  -11.22 -37.00 -30.00   99
  7  \w     34.00  98.00   1.00   10.00    --   11.30-178.00-180.00   64
  8  \w     -1.00  42.00   1.00   10.00    --   11.30-121.00-126.00   43
  9  \w    -61.00  39.00   1.00   10.00    --   11.30 -57.00-180.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0016968000
_diffrn_orient_matrix_UB_12      0.0425278000
_diffrn_orient_matrix_UB_13      -0.0032845000
_diffrn_orient_matrix_UB_21      -0.0053236000
_diffrn_orient_matrix_UB_22      0.0037664000
_diffrn_orient_matrix_UB_23      0.0349882000
_diffrn_orient_matrix_UB_31      0.0460759000
_diffrn_orient_matrix_UB_32      0.0019926000
_diffrn_orient_matrix_UB_33      0.0039182000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            106944
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.694
_diffrn_reflns_theta_min         3.352
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.574
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.512
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.646
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_preparation
'Red crystals were obtained from vapour-vapour diffusion of pentane into a DCM solution'
_exptl_crystal_recrystallization_method
'Red crystals were obtained from vapour-vapour diffusion of n-pentane into a DCM solution'
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.244
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+6.5612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0468
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5341
_reflns_number_total             6535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00876d1.cif
_cod_data_source_block           ram-16_scale
_cod_database_code               7701666
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H31 B1 N6 O2 W1'
_chemical_oxdiff_usercomment     'Red crystal blocks'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C17(H17)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              36413
_ins_header
;
TITL RAM-16_scale in Pbca 
REM Pbca (#61 in standard setting)
CELL 0.71073  15.284889  16.597387  20.053558  90.0000  90.0000  90.0000
ZERR    8.00   0.000183   0.000183   0.000249   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 B N O W
UNIT 192.00 248.00 8.00 48.00 16.00 8.00
TREF
HKLF 4
END
;
_olex2_date_sample_submission    2018-09-05
_olex2_submission_original_sample_id W(C3)(CO)2(Tp*)
_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 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.926