Bimetallic ethynylanthracenyl functionalised carbynes
Hill, Anthony; Frogley, Benjamin; Welsh, Steven S.; Chemical Communications  (2021) –; doi:10.1039/D1CC06142A

data_7129250
_publ_section_title
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 Bimetallic ethynylanthracenyl functionalised carbynes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06142A
_journal_year                    2021
_chemical_formula_moiety         'C74 H64 B2 N12 O4 W2'
_chemical_formula_sum            'C74 H64 B2 N12 O4 W2'
_chemical_formula_weight         1574.69
_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     iterative
_audit_creation_date             2020-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-21 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.982(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.7180(16)
_cell_length_b                   9.4131(4)
_cell_length_c                   18.4744(16)
_cell_measurement_reflns_used    5397
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.3750
_cell_measurement_theta_min      3.9670
_cell_volume                     3637.1(5)
_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    'olex2.solve (Bourhis et al., 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 0.992
_diffrn_measured_fraction_theta_max 0.814
_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    -42.00  40.00   1.00   48.00    --   12.97 -77.00 -60.00   82
  2  \w     51.00  85.00   1.00   48.00    --   12.97 178.00  90.00   34
  3  \w    -39.00  42.00   1.00   48.00    --   12.97 -19.00  30.00   81
;
_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      0.0283781000
_diffrn_orient_matrix_UB_12      0.0363363000
_diffrn_orient_matrix_UB_13      0.0235891000
_diffrn_orient_matrix_UB_21      -0.0185059000
_diffrn_orient_matrix_UB_22      0.0522834000
_diffrn_orient_matrix_UB_23      0.0091180000
_diffrn_orient_matrix_UB_31      0.0016061000
_diffrn_orient_matrix_UB_32      -0.0402490000
_diffrn_orient_matrix_UB_33      0.0331990000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.814
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14153
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.814
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.297
_diffrn_reflns_theta_min         3.252
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.215
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80099
_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    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             1564
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.033
_refine_diff_density_max         3.071
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         7366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0423P)^2^+3.5084P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5551
_reflns_number_total             7366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06142a2.cif
_cod_data_source_block           Compound_8
_cod_database_code               7129250
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C74 H60 B2 N12 O4 W2'
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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:
 C25(H25), C6(H6), C16(H16), C30(H30), C14(H14), C7(H7), C13(H13), C21(H21),
 C15(H15), C22(H22), C9(H9), C8(H8), C35(H35)
2.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C33(H33A,H33B,
 H33C), C32(H32A,H32B,H32C), C37(H37A,H37B,H37C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64240
_shelx_fab_checksum              58207
_ins_header
;
TITL BF125D2a_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  22.717998   9.413102  18.474442  90.0000 112.9821  90.0000
ZERR    2.00   0.001641   0.000410   0.001585   0.0000   0.0097   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O W
UNIT 148.00 120.00 4.00 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 1.260
_oxdiff_exptl_absorpt_empirical_full_min 0.786