Tetrel and pnictogen functionalised propargylidynes.
Manzano, Richard A.; Hill, Anthony F.; Georgelin, Rosemary L.; Chemical communications (Cambridge, England) 56 (2020) 14597–14600; doi:10.1039/d0cc06196d

data_7127723
_publ_section_title
;
 Tetrel and pnictogen functionalised propargylidynes.
;
_journal_issue                   93
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              14597
_journal_page_last               14600
_journal_paper_doi               10.1039/d0cc06196d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C32 H35 B2 N6 O2 P W, C H2 Cl2'
_chemical_formula_sum            'C33 H37 B2 Cl2 N6 O2 P W'
_chemical_formula_weight         857.02
_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
_audit_creation_date             2020-09-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-09-12 deposited with the CCDC.	2020-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.3819(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6458(2)
_cell_length_b                   13.04801(14)
_cell_length_c                   19.0700(3)
_cell_measurement_reflns_used    36379
_cell_measurement_temperature    170(30)
_cell_measurement_theta_max      29.6630
_cell_measurement_theta_min      3.6790
_cell_volume                     3559.48(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170(30)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3744
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_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    -39.00  62.00   1.00   35.00    --  -11.22  57.00 150.00  101
  2  \w    -20.00  30.00   1.00   35.00    --  -11.22 -99.00 150.00   50
  3  \w    -83.00  17.00   1.00   35.00    --  -11.22 -57.00   0.00  100
  4  \w    -36.00  63.00   1.00   35.00    --  -11.22  37.00  60.00   99
  5  \w    -20.00  30.00   1.00   35.00    --  -11.22 -99.00-180.00   50
  6  \w    -91.00  30.00   1.00   35.00    --  -11.22 -19.00 -90.00  121
  7  \w     34.00  98.00   1.00   35.00    --   11.30-178.00  30.00   64
  8  \w    -20.00  30.00   1.00   35.00    --  -11.22 -99.00-150.00   50
  9  \w    -71.00 -41.00   1.00   35.00    --  -11.22 132.00-148.00   30
 10  \w    -86.00  13.00   1.00   35.00    --  -11.22 -37.00  90.00   99
;
_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      0.0070142000
_diffrn_orient_matrix_UB_12      0.0037374000
_diffrn_orient_matrix_UB_13      0.0378787000
_diffrn_orient_matrix_UB_21      -0.0472961000
_diffrn_orient_matrix_UB_22      -0.0139937000
_diffrn_orient_matrix_UB_23      -0.0020443000
_diffrn_orient_matrix_UB_31      0.0131044000
_diffrn_orient_matrix_UB_32      -0.0524159000
_diffrn_orient_matrix_UB_33      0.0032554000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            71493
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.226
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.480
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.073
_refine_diff_density_max         2.641
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0225P)^2^+7.6226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6510
_reflns_number_total             7266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc06196d2.cif
_cod_data_source_block           Compound_9
_cod_original_cell_volume        3559.49(8)
_cod_database_code               7127723
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 B2 N6 O2 W1'
_chemical_oxdiff_usercomment     'Grown from DCM-pentane vdiffusion'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B)
2.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C25(H25), C30(H30), C7(H7), C8(H8), C9(H9), C17(H17), C13(H13),
 C14(H14), C10(H10), C11(H11), C16(H16), C15(H15)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C18(H18A,H18B,H18C), C28(H28A,H28B,H28C), C22(H22A,H22B,
 H22C), C32(H32A,H32B,H32C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              40638
_ins_header
;
TITL RAM-24a_scalefilt in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  14.645805  13.048013  19.070010  90.0000 102.3819  90.0000
ZERR    4.00   0.000201   0.000137   0.000252   0.0000   0.0013   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O W
UNIT 120.00 120.00 8.00 24.00 8.00 4.00
TREF
HKLF 4
END
;
_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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.859