Symmetric and Non-symmetric Anthracen-diyl Bis(alkylidynes)
Hill, Anthony; Frogley, Benjamin; Welsh, Steven S.; Dalton Transactions  (2021) –; doi:10.1039/D1DT02537F

data_7708364
_publ_section_title
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 Symmetric and Non-symmetric Anthracen-diyl Bis(alkylidynes)
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02537F
_journal_year                    2021
_chemical_formula_moiety         'C26 H18 B Br N6 O2 W'
_chemical_formula_sum            'C26 H18 B Br N6 O2 W'
_chemical_formula_weight         721.03
_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     dual
_audit_creation_date             2020-12-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6219)
;
_audit_update_record
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2021-04-13 deposited with the CCDC.	2021-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.750(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7252(7)
_cell_length_b                   10.8608(3)
_cell_length_c                   14.7832(7)
_cell_measurement_reflns_used    11584
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      29.5250
_cell_measurement_theta_min      3.7740
_cell_volume                     2418.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.831
_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    -86.00  13.00   1.00    7.50    --  -11.30 -37.00 -90.00   99
  2  \w    -12.00  16.00   1.00    7.50    --  -11.30 -99.00  60.00   28
  3  \w    -81.00  16.00   1.00    7.50    --  -11.30 -57.00 150.00   97
  4  \w    -23.00  64.00   1.00    7.50    --  -11.30  34.00  80.00   87
;
_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      -0.0206389000
_diffrn_orient_matrix_UB_12      -0.0290662000
_diffrn_orient_matrix_UB_13      0.0273438000
_diffrn_orient_matrix_UB_21      -0.0006449000
_diffrn_orient_matrix_UB_22      -0.0565408000
_diffrn_orient_matrix_UB_23      -0.0243208000
_diffrn_orient_matrix_UB_31      0.0423149000
_diffrn_orient_matrix_UB_32      -0.0149697000
_diffrn_orient_matrix_UB_33      0.0386943000
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.831
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21280
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.831
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.932
_diffrn_reflns_theta_min         3.590
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.088
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0139P)^2^+3.6082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0472
_refine_ls_wR_factor_ref         0.0502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5117
_reflns_number_total             5834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02537f2.cif
_cod_data_source_block           Compound_1b
_cod_original_cell_volume        2418.69(19)
_cod_database_code               7708364
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C26 H18 B Br N6 O2 W'
_chemical_oxdiff_usercomment     'DCM/MeOH RT'
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C6(H6), C26(H26), C16(H16), C19(H19), C21(H21), C18(H18),
 C13(H13), C15(H15), C7(H7), C20(H20), C14(H14), C22(H22), C23(H23), C9(H9),
 C8(H8)
;
_shelx_res_checksum              16662
_shelx_hkl_checksum              17565
_ins_header
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TITL BF121B3hemi_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  16.725227  10.860766  14.783175  90.0000 115.7502  90.0000
ZERR    4.00   0.000720   0.000349   0.000680   0.0000   0.0053   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O Br W
UNIT 104.00 72.00 4.00 24.00 8.00 4.00 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 1.699
_oxdiff_exptl_absorpt_empirical_full_min 0.703