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

data_7129248
_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         'C34 H31 B N6 O2 W'
_chemical_formula_sum            'C34 H31 B N6 O2 W'
_chemical_formula_weight         750.31
_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   geom
_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
;
2021-04-21 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.209(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9069(11)
_cell_length_b                   9.5403(5)
_cell_length_c                   18.2277(8)
_cell_measurement_reflns_used    5570
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.7440
_cell_measurement_theta_min      3.8220
_cell_volume                     3065.2(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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.830
_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      3.00  79.00   1.00   19.00    --   15.65  38.00 -60.00   76
  2  \w    -47.00  30.00   1.00   19.00    --   15.65 -57.00 120.00   77
  3  \w    -34.00   9.00   1.00   19.00    --  -16.36 -77.00 -90.00   43
;
_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      0.0286827000
_diffrn_orient_matrix_UB_12      0.0404446000
_diffrn_orient_matrix_UB_13      0.0279836000
_diffrn_orient_matrix_UB_21      -0.0184982000
_diffrn_orient_matrix_UB_22      0.0624429000
_diffrn_orient_matrix_UB_23      -0.0182797000
_diffrn_orient_matrix_UB_31      -0.0213232000
_diffrn_orient_matrix_UB_32      0.0003094000
_diffrn_orient_matrix_UB_33      0.0249678000
_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  0.0233
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.830
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12748
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.830
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.374
_diffrn_reflns_theta_min         3.412
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.810
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72894
_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    1.626
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.115
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         6997
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+2.0108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5563
_reflns_number_total             6997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06142a2.cif
_cod_data_source_block           Compound_5
_cod_database_code               7129248
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C34 H31 B N6 O2 W'
_chemical_oxdiff_usercomment     d/m
_reflns_odcompleteness_completeness 99.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C17A)=Sof(C12A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=Sof(H15A)=Sof(C13A)=
 Sof(H13A)=Sof(C14A)=Sof(H14A)=1-FVAR(1)
 Sof(C17)=Sof(C12)=Sof(C15)=Sof(H15)=Sof(C13)=Sof(H13)=Sof(C16)=Sof(H16)=
 Sof(C14)=Sof(H14)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 B1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C7(H7), C27(H27), C8(H8), C22(H22), C32(H32), C15(H15),
 C13(H13), C16(H16), C16A(H16A), C14(H14), C15A(H15A), C13A(H13A), C14A(H14A)
3.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C), C24(H24A,H24B,
 H24C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C)
3.d :
 C19(H19)
;
_shelx_res_checksum              93709
_ins_header
;
TITL BF123A_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  18.906888   9.540312  18.227677  90.0000 111.2092  90.0000
ZERR    4.00   0.001122   0.000513   0.000815   0.0000   0.0057   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O W
UNIT 136.00 124.00 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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.630