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

data_7708369
_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         'C29 H24 B Br N6 O2 S3 W'
_chemical_formula_sum            'C29 H24 B Br N6 O2 S3 W'
_chemical_formula_weight         859.29
_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             2021-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-08 deposited with the CCDC.	2021-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.208(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4825(3)
_cell_length_b                   15.3301(4)
_cell_length_c                   22.6473(7)
_cell_measurement_reflns_used    5911
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.3270
_cell_measurement_theta_min      3.9150
_cell_volume                     3287.03(17)
_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 (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 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.983
_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   -105.00  -8.00   1.00    1.00    --  -35.78 -19.00 -30.00   97
  2  \w    -96.00 -22.00   1.00    1.00    --  -35.78 -57.00  90.00   74
  3  \w    -99.00 -20.00   1.00    1.00    --  -35.78 -57.00 -90.00   79
  4  \w    -96.00 -20.00   1.00    1.00    --  -35.78 -57.00-180.00   76
  5  \w    -87.00 -36.00   1.00    1.00    --  -35.78 125.00 -30.00   51
  6  \w     43.00  85.00   1.00    1.00    --   35.78-125.00-120.00   42
  7  \w     35.00 117.00   1.00    3.00    --  105.15 -30.00 -60.00   82
  8  \w     38.00 132.00   1.00    3.00    --  105.15 -77.00  60.00   94
  9  \w     35.00 126.00   1.00    3.00    --  105.15 -30.00  30.00   91
 10  \w     42.00 121.00   1.00    3.00    --  105.15 -45.00-180.00   79
 11  \w     88.00 174.00   1.00    3.00    --  105.15  45.00 -30.00   86
 12  \w     35.00 109.00   1.00    3.00    --  105.15-111.00-120.00   74
 13  \w     60.00 131.00   1.00    3.00    --  105.15 -77.00-120.00   71
 14  \w     42.00 106.00   1.00    3.00    --  105.15 -95.00  30.00   64
 15  \w     67.00 176.00   1.00    3.00    --  105.15  15.00 -90.00  109
;
_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      0.0060018000
_diffrn_orient_matrix_UB_12      -0.0264505000
_diffrn_orient_matrix_UB_13      0.0657315000
_diffrn_orient_matrix_UB_21      -0.1270227000
_diffrn_orient_matrix_UB_22      0.0597659000
_diffrn_orient_matrix_UB_23      0.0100254000
_diffrn_orient_matrix_UB_31      -0.1016103000
_diffrn_orient_matrix_UB_32      -0.0762939000
_diffrn_orient_matrix_UB_33      -0.0148649000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17991
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.652
_diffrn_reflns_theta_min         3.910
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.018
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39436
_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            orange
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_description       prism
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.075
_refine_diff_density_max         3.075
_refine_diff_density_min         -1.647
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0828P)^2^+17.7795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1442
_refine_ls_wR_factor_ref         0.1590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4769
_reflns_number_total             6205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02537f2.cif
_cod_data_source_block           Compound_1c
_cod_database_code               7708369
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C29 H24 B Br N6 O2 S3 W'
_chemical_oxdiff_usercomment     'DCM/Petrol (40-60) Vap. Diff.'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C27(H27), C20(H20), C6(H6), C21(H21), C15(H15), C14(H14), C23(H23), C16(H16),
 C24(H24), C7(H7), C28(H28), C13(H13), C8(H8), C9(H9)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              35675
_shelx_hkl_checksum              54939
_shelx_fab_checksum              62430
_ins_header
;
TITL SW171A_2_hemi_scale_v2 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 1.54184   9.482535  15.330085  22.647263  90.0000  93.2081  90.0000
ZERR    4.00   0.000278   0.000436   0.000690   0.0000   0.0026   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O S Br W
UNIT 116.00 96.00 4.00 24.00 8.00 12.00 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 2.179
_oxdiff_exptl_absorpt_empirical_full_min 0.702