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_7701668
_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         'C38 H37 B N6 O2 Si W'
_chemical_formula_sum            'C38 H37 B N6 O2 Si W'
_chemical_formula_weight         832.48
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-09-12
_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                 95.280(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9396(9)
_cell_length_b                   12.8019(8)
_cell_length_c                   19.6756(10)
_cell_measurement_reflns_used    5563
_cell_measurement_temperature    149.99(11)
_cell_measurement_theta_max      28.0440
_cell_measurement_theta_min      3.7910
_cell_volume                     3997.9(4)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(11)
_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 0.998
_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    -80.00  14.00   1.00  290.00    --  -11.22 -57.00  90.00   94
  2  \w     -5.00  30.00   1.00  290.00    --  -11.22  57.00-150.00   35
  3  \w    -92.00 -34.00   1.00  290.00    --  -11.22 178.00-150.00   58
  4  \w     70.00  95.00   1.00  290.00    --   11.46 178.00 -30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0424443000
_diffrn_orient_matrix_UB_12      0.0018076000
_diffrn_orient_matrix_UB_13      0.0144696000
_diffrn_orient_matrix_UB_21      -0.0053583000
_diffrn_orient_matrix_UB_22      -0.0488774000
_diffrn_orient_matrix_UB_23      0.0159641000
_diffrn_orient_matrix_UB_31      0.0130070000
_diffrn_orient_matrix_UB_32      -0.0259114000
_diffrn_orient_matrix_UB_33      -0.0291151000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21582
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.270
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.957
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98209
_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    1.383
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
_exptl_crystal_recrystallization_method
'Grown from slow evaporationg of a chloroform/ethanol solution at 0 degrees celcius'
_exptl_crystal_size_max          0.152
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.384
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         8152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0309P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5970
_reflns_number_total             8152
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00876d1.cif
_cod_data_source_block           platon_sq
_cod_database_code               7701668
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C40 H40 B1 Cl4 N6 O2 Si1 W'
_chemical_oxdiff_usercomment
'Grown from slow evaporation of DCM/EtOH solution at 0 degrees celcius'
_shelx_estimated_absorpt_t_max   0.800
_shelx_estimated_absorpt_t_min   0.662
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C25(H25), C19(H19), C20(H20), C31(H31), C23(H23), C22(H22),
 C21(H21), C7(H7), C14(H14), C17(H17), C9(H9), C8(H8), C10(H10), C11(H11),
 C15(H15), C16(H16), C13(H13)
2.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C34(H34A,H34B,H34C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              16034
_shelx_fab_checksum              89746
_ins_header
;
TITL RAM-40scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  15.939619  12.801930  19.675554  90.0000  95.2799  90.0000
ZERR    4.00   0.000943   0.000834   0.000989   0.0000   0.0057   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O Si Cl W
UNIT 160.00 160.00 4.00 24.00 8.00 4.00 16.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_original_sample_id RAM-40
_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 1.077
_oxdiff_exptl_absorpt_empirical_full_min 0.955