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

data_7708362
_publ_section_title
;
 Symmetric and Non-symmetric Anthracen-diyl Bis(alkylidynes)
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02537F
_journal_year                    2021
_chemical_formula_moiety         'C32 H30 B Br N6 O2 W'
_chemical_formula_sum            'C32 H30 B Br N6 O2 W'
_chemical_formula_weight         805.19
_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   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
;
2021-04-13 deposited with the CCDC.	2021-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                77.296(2)
_cell_angle_beta                 83.660(2)
_cell_angle_gamma                72.785(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4587(2)
_cell_length_b                   11.4422(2)
_cell_length_c                   13.8472(3)
_cell_measurement_reflns_used    11649
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.6250
_cell_measurement_theta_min      5.1190
_cell_volume                     1542.29(6)
_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 2014/5 (Sheldrick, 2014)'
_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 0.999
_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    -29.00  54.00   1.00    1.00    --   37.08 -57.00-120.00   83
  2  \w     60.00  90.00   1.00    1.00    --   37.08  19.00 120.00   30
  3  \w     51.00  90.00   1.00    1.00    --   37.08-125.00 120.00   39
  4  \w     17.00  44.00   1.00    1.00    --   37.08 -77.00  30.00   27
  5  \w     42.00  75.00   1.00    1.00    --   37.08 -99.00 -30.00   33
  6  \w     19.00 103.00   1.00    1.00    --   37.08  38.00  30.00   84
  7  \w     19.00 100.00   1.00    1.00    --   37.08  38.00-120.00   81
  8  \w      4.00  31.00   1.00    1.00    --   37.08 -19.00  90.00   27
  9  \w     11.00  36.00   1.00    1.00    --   37.08  19.00 120.00   25
 10  \w     19.00  78.00   1.00    1.00    --   37.08  38.00-180.00   59
 11  \w     66.00  95.00   1.00    1.00    --   37.08  57.00 -60.00   29
 12  \w     28.00  87.00   1.00    1.00    --   37.08  57.00  90.00   59
 13  \w    -30.00  -3.00   1.00    1.00    --   37.08 -19.00  90.00   27
 14  \w     51.00  89.00   1.00    1.00    --   37.08-125.00-120.00   38
 15  \w     52.00  99.00   1.00    1.00    --  111.00-111.00   0.00   47
 16  \w     92.00 130.00   1.00    1.00    --  111.00 -64.00 120.00   38
 17  \w     58.00 109.00   1.00    1.00    --  111.00 -38.00 -30.00   51
 18  \w     88.00 131.00   1.00    1.00    --  111.00  25.00-150.00   43
 19  \w     66.00 109.00   1.00    1.00    --  111.00-111.00 -60.00   43
 20  \w     81.00 108.00   1.00    1.00    --  111.00-111.00-120.00   27
 21  \w     42.00 100.00   1.00    1.00    --  111.00 -38.00  60.00   58
 22  \w    123.00 150.00   1.00    1.00    --  111.00 111.00  60.00   27
 23  \w     81.00 108.00   1.00    1.00    --  111.00-104.00  97.00   27
 24  \w     81.00 109.00   1.00    1.00    --  111.00-111.00  30.00   28
 25  \w    138.00 176.00   1.00    1.00    --  111.00  38.00   0.00   38
 26  \w    112.00 168.00   1.00    1.00    --  111.00  38.00  90.00   56
 27  \w    132.00 177.00   1.00    1.00    --  111.00  12.00 120.00   45
 28  \w    105.00 167.00   1.00    1.00    --  111.00 111.00-150.00   62
 29  \w     44.00 125.00   1.00    1.00    --  111.00 -50.00-120.00   81
 30  \w    131.00 175.00   1.00    1.00    --  111.00  64.00 -30.00   44
 31  \w    152.00 177.00   1.00    1.00    --  111.00  50.00  90.00   25
 32  \w     43.00  88.00   1.00    1.00    --  111.00-111.00 -90.00   45
 33  \w    100.00 157.00   1.00    1.00    --  111.00  50.00 150.00   57
 34  \w     42.00  87.00   1.00    1.00    --  111.00 -92.00-180.00   45
 35  \w    128.00 163.00   1.00    1.00    --  111.00  50.00 120.00   35
 36  \w     94.00 131.00   1.00    1.00    --  111.00  38.00  30.00   37
 37  \w     90.00 127.00   1.00    1.00    --  111.00 -50.00 150.00   37
 38  \w     44.00 101.00   1.00    1.00    --  111.00 -64.00   0.00   57
 39  \w    135.00 164.00   1.00    1.00    --  111.00  38.00  30.00   29
 40  \w     92.00 141.00   1.00    1.00    --  111.00  38.00 120.00   49
 41  \w     63.00  90.00   1.00    1.00    --  111.00 -77.00 -60.00   27
 42  \w     54.00  87.00   1.00    1.00    --  111.00 -50.00 150.00   33
 43  \w     78.00 103.00   1.00    1.00    --  111.00-111.00  60.00   25
 44  \w     67.00 106.00   1.00    1.00    --  111.00 -92.00  90.00   39
 45  \w     64.00 108.00   1.00    1.00    --  111.00-111.00-180.00   44
 46  \w     42.00  67.00   1.00    1.00    --  111.00-111.00-120.00   25
 47  \w     44.00 109.00   1.00    1.00    --  111.00-111.00  90.00   65
 48  \w     80.00 105.00   1.00    1.00    --  111.00 -92.00-150.00   25
 49  \w    145.00 170.00   1.00    1.00    --  111.00  50.00  60.00   25
 50  \w     95.00 129.00   1.00    1.00    --  111.00  38.00   0.00   34
 51  \w    143.00 175.00   1.00    1.00    --  111.00  25.00 -60.00   32
 52  \w    102.00 152.00   1.00    1.00    --  111.00  38.00  60.00   50
 53  \w    140.00 168.00   1.00    1.00    --  111.00  77.00  30.00   28
 54  \w     97.00 126.00   1.00    1.00    --  111.00 -64.00 -30.00   29
 55  \w     69.00 108.00   1.00    1.00    --  111.00-111.00 -30.00   39
 56  \w     61.00 107.00   1.00    1.00    --  111.00-111.00 150.00   46
 57  \w     60.00  99.00   1.00    1.00    --  111.00 -67.00 -33.64   39
;
_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      0.0909626000
_diffrn_orient_matrix_UB_12      0.0260969000
_diffrn_orient_matrix_UB_13      -0.0927493000
_diffrn_orient_matrix_UB_21      0.1245442000
_diffrn_orient_matrix_UB_22      -0.0758528000
_diffrn_orient_matrix_UB_23      0.0590906000
_diffrn_orient_matrix_UB_31      -0.0071499000
_diffrn_orient_matrix_UB_32      -0.1193197000
_diffrn_orient_matrix_UB_33      -0.0307149000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17784
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.877
_diffrn_reflns_theta_min         4.126
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56246
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         6200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0437P)^2^+0.6608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5920
_reflns_number_total             6200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02537f2.cif
_cod_data_source_block           Compound_1a
_cod_database_code               7708362
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 H26 B Br N6 O2 W'
_chemical_oxdiff_usercomment     'DCM/MeOH evap RT'
_reflns_odcompleteness_completeness 98.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C16(H16), C24(H24), C13(H13), C15(H15), C6(H6), C9(H9), C8(H8), C29(H29),
 C14(H14), C19(H19), C7(H7)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C21(H21A,H21B,H21C), C31(H31A,H31B,
 H31C), C27(H27A,H27B,H27C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              84822
_shelx_hkl_checksum              33234
_ins_header
;
TITL BF121A4_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.458698  11.442211  13.847159  77.2959  83.6602  72.7848
ZERR    2.00   0.000211   0.000213   0.000284   0.0017   0.0017   0.0017
LATT  1
SFAC C H B N O Br W
UNIT 64.00 52.00 2.00 12.00 4.00 2.00 2.00
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 1.807
_oxdiff_exptl_absorpt_empirical_full_min 0.708