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

data_7708370
_publ_section_title
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 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         'C52 H36 B2 Br2 N12 O4 Pd W2'
_chemical_formula_sum            'C52 H36 B2 Br2 N12 O4 Pd W2'
_chemical_formula_weight         1548.47
_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             2020-12-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
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2021-04-21 deposited with the CCDC.	2021-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.146(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5661(4)
_cell_length_b                   21.7317(7)
_cell_length_c                   22.2650(7)
_cell_measurement_reflns_used    7327
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      27.4940
_cell_measurement_theta_min      3.7380
_cell_volume                     5471.1(3)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.813
_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    -40.00  11.00   1.00   50.00    --   12.73 -77.00 -30.00   51
  2  \w    -13.00  52.00   1.00   50.00    --   12.73 -99.00-180.00   65
  3  \w      1.00  74.00   1.00   50.00    --   12.73  57.00 -90.00   73
;
_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      -0.0618803000
_diffrn_orient_matrix_UB_12      0.0002470000
_diffrn_orient_matrix_UB_13      -0.0120716000
_diffrn_orient_matrix_UB_21      0.0099359000
_diffrn_orient_matrix_UB_22      -0.0089128000
_diffrn_orient_matrix_UB_23      -0.0291366000
_diffrn_orient_matrix_UB_31      -0.0033613000
_diffrn_orient_matrix_UB_32      -0.0313890000
_diffrn_orient_matrix_UB_33      0.0081610000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.813
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            20915
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.230
_diffrn_reflns_theta_min         3.376
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.036
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86857
_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_colour_primary    red
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.044
_refine_diff_density_max         2.045
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         10985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0430P)^2^+10.2201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8784
_reflns_number_total             10985
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02537f2.cif
_cod_data_source_block           Compound_3a_CCDC1
_cod_database_code               7708370
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H36 B2 Br2 N12 O4 Pd W2'
_chemical_oxdiff_usercomment     c/e
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C47(H47), C49(H49), C21(H21), C25(H25), C6(H6), C24(H24),
 C26(H26), C52(H52), C50(H50), C48(H48), C46(H46), C22(H22), C19(H19), C23(H23),
  C42(H42), C51(H51), C32(H32), C44(H44), C16(H16), C45(H45), C7(H7), C33(H33),
 C13(H13), C34(H34), C9(H9), C8(H8), C39(H39), C15(H15), C35(H35), C40(H40),
 C41(H41), C14(H14)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              96304
_shelx_hkl_checksum              83882
_shelx_fab_checksum              58607
_ins_header
;
TITL BF124A2_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  11.566143  21.731707  22.264961  90.0000 102.1459  90.0000
ZERR    4.00   0.000418   0.000701   0.000721   0.0000   0.0033   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O Br Pd W
UNIT 208.00 144.00 8.00 48.00 16.00 8.00 4.00 8.00
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 1.155
_oxdiff_exptl_absorpt_empirical_full_min 0.900