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

data_7129247
_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
'C52 H63 Au B N6 O2 P W, C6 H12, 2(C0.75 H0.75 Cl2.25)'
_chemical_formula_sum            'C59.5 H76.5 Au B Cl4.5 N6 O2 P W'
_chemical_formula_weight         1489.97
_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             2020-12-16
_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                 114.172(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7071(9)
_cell_length_b                   16.1172(4)
_cell_length_c                   21.1538(9)
_cell_measurement_reflns_used    9292
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.6150
_cell_measurement_theta_min      3.7920
_cell_volume                     6440.9(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    '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 0.992
_diffrn_measured_fraction_theta_max 0.816
_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     -4.00  80.00   1.00   39.00    --   12.97  57.00 -60.00   84
  2  \w     -4.00  80.00   1.00   39.00    --   12.97  57.00  30.00   84
  3  \w    -12.00  13.00   1.00   39.00    --  -13.67 -77.00 -30.00   25
;
_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      0.0370581000
_diffrn_orient_matrix_UB_12      0.0053599000
_diffrn_orient_matrix_UB_13      0.0113341000
_diffrn_orient_matrix_UB_21      0.0041116000
_diffrn_orient_matrix_UB_22      -0.0016031000
_diffrn_orient_matrix_UB_23      0.0349744000
_diffrn_orient_matrix_UB_31      0.0044215000
_diffrn_orient_matrix_UB_32      -0.0436233000
_diffrn_orient_matrix_UB_33      0.0001356000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.816
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24626
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.258
_diffrn_reflns_theta_min         3.323
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.315
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55720
_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_colour_primary    orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       prism
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.026
_refine_diff_density_max         2.531
_refine_diff_density_min         -2.118
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         13019
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0270P)^2^+47.5082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9539
_reflns_number_total             13019
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06142a2.cif
_cod_data_source_block           Compound_6b
_cod_original_formula_sum        'C59.50 H76.50 Au B Cl4.50 N6 O2 P W'
_cod_database_code               7129247
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C52 H63 Au B N6 O2 P W'
_reflns_odcompleteness_completeness 99.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C60-Cl7 \\sim C60-Cl8 \\sim C60-Cl9 \\sim C60-Cl10 \\sim C60-Cl11 \\sim
C60-Cl12
 with sigma of 0.02
 C56-C57 \\sim C57-C58 \\sim C56-C57A \\sim C57A-C58
 with sigma of 0.02
 C53-C54 \\sim C54-C55 \\sim C53-C54A \\sim C54A-C55
 with sigma of 0.02
 C59-Cl1 \\sim C59-Cl2 \\sim C59-Cl3 \\sim C59-Cl4 \\sim C59-Cl5 \\sim C59-Cl6
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C57A \\sim C58 \\sim C53 \\sim C54 \\sim C54A \\sim C57 \\sim C55 \\sim C56:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
N5 \\sim N6 \\sim C33 \\sim C32 \\sim C31: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Cl3 \\sim Cl2 \\sim Cl1 \\sim Cl6 \\sim C59 \\sim Cl4 \\sim Cl5: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Cl7 \\sim Cl8 \\sim Cl9 \\sim Cl10 \\sim Cl11 \\sim Cl12: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 Cl7, C60, Cl8, Cl9, Cl10, Cl11, Cl12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, Cl3, C59, Cl1, Cl6, Cl4, Cl5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(H59)+Sof(Cl6)+Sof(Cl2)+Sof(Cl5)]+1*[Sof(Cl4)+Sof(Cl3)+Sof(Cl1)+
 Sof(H59A)]=0.75 with esd of 0.001
 1*[Sof(Cl11)+Sof(Cl9)+Sof(Cl7)+Sof(H60)]+1*[Sof(Cl10)+Sof(Cl12)+Sof(Cl8)+
 Sof(H60A)]=0.75 with esd of 0.001
 Sof(H59)=Sof(Cl6)=Sof(Cl2)=Sof(Cl5)=FVAR(1)
 Sof(Cl11)=Sof(Cl9)=Sof(Cl7)=Sof(H60)=FVAR(2)
 Sof(Cl4)=Sof(Cl3)=Sof(Cl1)=Sof(H59A)=FVAR(3)
 Sof(Cl10)=Sof(Cl12)=Sof(Cl8)=Sof(H60A)=FVAR(4)
 Sof(H53C)=Sof(H53D)=Sof(H58C)=Sof(H58D)=Sof(H55C)=Sof(H55D)=Sof(H56C)=
 Sof(H56D)=Sof(C57A)=Sof(H57C)=Sof(H57D)=Sof(C54A)=Sof(H54C)=Sof(H54D)=1-FVAR(5)
 Sof(H53A)=Sof(H53B)=Sof(H58A)=Sof(H58B)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(C57)=
 Sof(H57A)=Sof(H57B)=Sof(H55A)=Sof(H55B)=Sof(H56A)=Sof(H56B)=FVAR(5)
 Fixed Sof: C59(0.75) C60(0.75)
6.a Ternary CH refined with riding coordinates:
 C41(H41), C47(H47), C35(H35), C59(H59A), C59(H59), C60(H60), C60(H60A)
6.b Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C52(H52A,H52B), C45(H45A,H45B), C44(H44A,H44B), C42(H42A,
 H42B), C48(H48A,H48B), C46(H46A,H46B), C40(H40A,H40B), C38(H38A,H38B),
 C43(H43A,H43B), C51(H51A,H51B), C39(H39A,H39B), C49(H49A,H49B), C37(H37A,H37B),
  C50(H50A,H50B), C53(H53A,H53B), C53(H53C,H53D), C58(H58A,H58B), C58(H58C,
 H58D), C54(H54A,H54B), C57(H57A,H57B), C55(H55A,H55B), C55(H55C,H55D),
 C56(H56A,H56B), C56(H56C,H56D), C57A(H57C,H57D), C54A(H54C,H54D)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C32(H32), C16(H16), C7(H7), C27(H27), C14(H14), C13(H13), C15(H15),
 C9(H9), C8(H8), C22(H22)
6.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C25(H25A,H25B,H25C), C24(H24A,H24B,
 H24C), C20(H20A,H20B,H20C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              97856
_ins_header
;
TITL BF123Ca_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  20.707086  16.117165  21.153809  90.0000 114.1720  90.0000
ZERR    6.00   0.000872   0.000429   0.000928   0.0000   0.0053   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O P W Au
UNIT 312.00 378.00 6.00 36.00 12.00 6.00 6.00 6.00
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 1.564
_oxdiff_exptl_absorpt_empirical_full_min 0.740