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

data_7129246
_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         'C37 H39 B N6 O2 Si W, C H Cl3'
_chemical_formula_sum            'C38 H40 B Cl3 N6 O2 Si W'
_chemical_formula_weight         941.86
_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             2020-12-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6219)
;
_audit_update_record
;
2021-04-21 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.277(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5631(4)
_cell_length_b                   10.4599(3)
_cell_length_c                   26.8791(9)
_cell_measurement_reflns_used    16749
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.6050
_cell_measurement_theta_min      3.5940
_cell_volume                     4028.8(2)
_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 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.863
_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    -14.00  30.00   1.00   12.00    --  -11.30 -99.00 -60.00   44
  2  \w     39.00  97.00   1.00   12.00    --   11.61 178.00 120.00   58
  3  \w    -19.00  33.00   1.00   12.00    --   11.61 -77.00 -30.00   52
  4  \w    -42.00  41.00   1.00   12.00    --   11.61 -77.00 120.00   83
  5  \w    -57.00  -9.00   1.00   12.00    --   11.61 -57.00  90.00   48
  6  \w      1.00  82.00   1.00   12.00    --   11.61  57.00-120.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0188803000
_diffrn_orient_matrix_UB_12      0.0424268000
_diffrn_orient_matrix_UB_13      -0.0197780000
_diffrn_orient_matrix_UB_21      -0.0123473000
_diffrn_orient_matrix_UB_22      -0.0527928000
_diffrn_orient_matrix_UB_23      -0.0163967000
_diffrn_orient_matrix_UB_31      -0.0440478000
_diffrn_orient_matrix_UB_32      -0.0033947000
_diffrn_orient_matrix_UB_33      0.0077101000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            40625
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.017
_diffrn_reflns_theta_min         3.419
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.137
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65077
_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    1.553
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.511
_exptl_crystal_size_mid          0.352
_exptl_crystal_size_min          0.157
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         10171
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0247P)^2^+12.7856P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0881
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7793
_reflns_number_total             10171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06142a2.cif
_cod_data_source_block           Compound_2a
_cod_database_code               7129246
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37 H39 B N6 O2 Si W'
_chemical_oxdiff_usercomment     c/e
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 C38-Cl1 \\sim C38-Cl2 \\sim C38-Cl3 \\sim C38A-Cl1A \\sim C38A-Cl2A \\sim
C38A-Cl3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C38A) = Uanis(C38)
Uanis(Cl3A) = Uanis(Cl1)
Uanis(Cl2A) = Uanis(Cl2)
Uanis(Cl1A) = Uanis(Cl3)
4. Others
 Sof(Cl3A)=Sof(Cl2A)=Sof(C38A)=Sof(H38A)=Sof(Cl1A)=1-FVAR(1)
 Sof(Cl2)=Sof(Cl3)=Sof(C38)=Sof(H38)=Sof(Cl1)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C38(H38), C38A(H38A)
5.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C14(H14), C35(H35), C7(H7), C13(H13), C6(H6), C25(H25), C30(H30),
 C15(H15), C8(H8), C9(H9)
5.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C33(H33A,H33B,H33C), C20(H20A,H20B,H20C), C28(H28A,H28B,
 H28C), C22(H22A,H22B,H22C), C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C32(H32A,
 H32B,H32C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              18702
_ins_header
;
TITL BF122A2_scale in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  14.563120  10.459875  26.879063  90.0000 100.2772  90.0000
ZERR    4.00   0.000388   0.000315   0.000863   0.0000   0.0026   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H B N O Si W
UNIT 148.00 156.00 4.00 24.00 8.00 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 1.464
_oxdiff_exptl_absorpt_empirical_full_min 0.791