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

data_7708367
_publ_section_title
;
 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         'C44 H40 B2 Mo N12 O4 W, 1.5(C H Cl3)'
_chemical_formula_sum            'C45.5 H41.5 B2 Cl4.5 Mo N12 O4 W'
_chemical_formula_weight         1281.34
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-13 deposited with the CCDC.	2021-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                63.6320(10)
_cell_angle_beta                 68.5650(10)
_cell_angle_gamma                69.6860(10)
_cell_formula_units_Z            4
_cell_length_a                   17.0117(2)
_cell_length_b                   18.7902(2)
_cell_length_c                   19.9613(2)
_cell_measurement_reflns_used    55302
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5790
_cell_measurement_theta_min      4.8110
_cell_volume                     5189.06(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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     27.00  52.00   1.00    1.50    --   36.95-125.00  30.00   25
  2  \w     56.00  90.00   1.00    1.50    --   36.95-125.00  30.00   34
  3  \w     30.00  81.00   1.00    1.50    --   36.95-125.00 -30.00   51
  4  \w      3.00  28.00   1.00    1.50    --   36.95  90.00-151.83   25
  5  \w      4.00  29.00   1.00    1.50    --   36.95  88.00  16.35   25
  6  \w     56.00 104.00   1.00    1.50    --   36.95  57.00   0.00   48
  7  \w     61.00 105.00   1.00    1.50    --   36.95  38.00 120.00   44
  8  \w     22.00  49.00   1.00    1.50    --   36.95  57.00-180.00   27
  9  \w     25.00  53.00   1.00    1.50    --   36.95  38.00 -60.00   28
 10  \w      4.00  30.00   1.00    1.50    --   36.95  88.00 145.83   26
 11  \w     64.00  89.00   1.00    1.50    --   36.95  57.00 -60.00   25
 12  \w     14.00  84.00   1.00    1.50    --   36.95  72.00  28.10   70
 13  \w     60.00  87.00   1.00    1.50    --   36.95-125.00  90.00   27
 14  \w     61.00  91.00   1.00    1.50    --   36.95  57.00-120.00   30
 15  \w      5.00  30.00   1.00    1.50    --   36.95  88.00  58.17   25
 16  \w    -31.00  30.00   1.00    1.50    --   36.95 -38.00 -90.00   61
 17  \w     35.00  85.00   1.00    1.50    --   36.95   0.00-150.00   50
 18  \w     55.00 101.00   1.00    1.50    --   36.95  57.00-180.00   46
 19  \w     20.00  48.00   1.00    1.50    --   36.95  57.00 -90.00   28
 20  \w     39.00  74.00   1.00    1.50    --   36.95 -99.00-180.00   35
 21  \w     21.00  48.00   1.00    1.50    --   36.95  57.00   0.00   27
 22  \w    -28.00  52.00   1.00    1.50    --   36.95 -57.00-180.00   80
 23  \w     28.00  55.00   1.00    1.50    --   36.95-125.00  90.00   27
 24  \w      5.00  56.00   1.00    1.50    --   36.95 -38.00 -60.00   51
 25  \w     14.00  61.00   1.00    1.50    --   36.95  72.00 -57.45   47
 26  \w    -21.00  39.00   1.00    1.50    --   36.95 -57.00 120.00   60
 27  \w      8.00  94.00   1.00    1.50    --   36.95  19.00 120.00   86
 28  \w     11.00  42.00   1.00    1.50    --   36.95  77.00 -31.96   31
 29  \w    -32.00  43.00   1.00    1.50    --   36.95 -38.00  30.00   75
 30  \w     21.00  47.00   1.00    1.50    --   36.95  57.00-120.00   26
 31  \w     48.00 105.00   1.00    1.50    --   36.95  38.00-120.00   57
 32  \w     22.00  57.00   1.00    1.50    --   36.95  57.00 -60.00   35
 33  \w      9.00  37.00   1.00    1.50    --   36.95  79.00 113.09   28
 34  \w    -28.00  44.00   1.00    1.50    --   36.95 -57.00 150.00   72
 35  \w     19.00  55.00   1.00    1.50    --   36.95  38.00 120.00   36
 36  \w     27.00  82.00   1.00    1.50    --   36.95-125.00 120.00   55
 37  \w    -27.00  -1.00   1.00    1.50    --   36.95   0.00-150.00   26
 38  \w     68.00  93.00   1.00    1.50    --   36.95  72.00 -57.45   25
 39  \w     81.00 106.00   1.00    1.50    --   36.95  38.00 -60.00   25
 40  \w     54.00  89.00   1.00    1.50    --   36.95  57.00 -90.00   35
 41  \w     54.00  95.00   1.00    1.50    --   36.95  38.00-180.00   41
 42  \w     21.00  49.00   1.00    1.50    --   36.95  38.00-180.00   28
 43  \w     91.00 119.00   1.00    6.50    --  111.00  64.00-120.00   28
 44  \w    134.00 161.00   1.00    6.50    --  111.00  64.00  90.00   27
 45  \w     93.00 118.00   1.00    6.50    --  111.00  38.00  60.00   25
 46  \w     91.00 117.00   1.00    6.50    --  111.00  64.00  90.00   26
 47  \w     94.00 120.00   1.00    6.50    --  111.00  50.00 -90.00   26
 48  \w     92.00 137.00   1.00    6.50    --  111.00  38.00 -60.00   45
 49  \w     92.00 118.00   1.00    6.50    --  111.00  63.00   5.26   26
 50  \w     61.00  99.00   1.00    6.50    --  111.00 -92.00  30.00   38
 51  \w     41.00 109.00   1.00    6.50    --  111.00-111.00 120.00   68
 52  \w     94.00 145.00   1.00    6.50    --  111.00  50.00-180.00   51
 53  \w     92.00 118.00   1.00    6.50    --  111.00  38.00   0.00   26
 54  \w     94.00 125.00   1.00    6.50    --  111.00  50.00-120.00   31
 55  \w     91.00 117.00   1.00    6.50    --  111.00  64.00   0.00   26
 56  \w     91.00 130.00   1.00    6.50    --  111.00  64.00  30.00   39
 57  \w    135.00 178.00   1.00    6.50    --  111.00  64.00  30.00   43
 58  \w     94.00 120.00   1.00    6.50    --  111.00  50.00 150.00   26
 59  \w     43.00 109.00   1.00    6.50    --  111.00-111.00-120.00   66
 60  \w    102.00 127.00   1.00    6.50    --  111.00 -50.00 -90.00   25
 61  \w     86.00 122.00   1.00    6.50    --  111.00  25.00 -60.00   36
 62  \w     60.00 105.00   1.00    6.50    --  111.00-122.00  34.00   45
 63  \w     86.00 128.00   1.00    6.50    --  111.00  25.00 -90.00   42
 64  \w     50.00 109.00   1.00    6.50    --  111.00-111.00 -90.00   59
 65  \w     94.00 121.00   1.00    6.50    --  111.00  50.00  90.00   27
 66  \w     94.00 121.00   1.00    6.50    --  111.00  50.00 120.00   27
 67  \w     92.00 119.00   1.00    6.50    --  111.00  38.00-150.00   27
 68  \w     94.00 120.00   1.00    6.50    --  111.00  50.00   0.00   26
 69  \w    145.00 171.00   1.00    6.50    --  111.00  25.00  30.00   26
 70  \w    130.00 171.00   1.00    6.50    --  111.00  64.00  60.00   41
 71  \w    135.00 175.00   1.00    6.50    --  111.00  73.00 -35.25   40
 72  \w    129.00 177.00   1.00    6.50    --  111.00  50.00 -30.00   48
 73  \w     94.00 120.00   1.00    6.50    --  111.00  50.00 -30.00   26
 74  \w     91.00 116.00   1.00    6.50    --  111.00  64.00  60.00   25
 75  \w     94.00 120.00   1.00    6.50    --  111.00  50.00  60.00   26
 76  \w     93.00 118.00   1.00    6.50    --  111.00  38.00 -90.00   25
 77  \w     92.00 118.00   1.00    6.50    --  111.00  38.00-120.00   26
 78  \w    151.00 177.00   1.00    6.50    --  111.00  50.00-150.00   26
 79  \w     86.00 121.00   1.00    6.50    --  111.00  25.00  60.00   35
 80  \w    132.00 178.00   1.00    6.50    --  111.00  64.00-180.00   46
 81  \w     94.00 120.00   1.00    6.50    --  111.00  50.00-150.00   26
 82  \w     87.00 112.00   1.00    6.50    --  111.00  25.00 -30.00   25
 83  \w    127.00 153.00   1.00    6.50    --  111.00  25.00  90.00   26
 84  \w     91.00 117.00   1.00    6.50    --  111.00  64.00-180.00   26
 85  \w     86.00 122.00   1.00    6.50    --  111.00  25.00  90.00   36
 86  \w     87.00 154.00   1.00    6.50    --  111.00  25.00 120.00   67
 87  \w    135.00 177.00   1.00    6.50    --  111.00  64.00 120.00   42
 88  \w     92.00 130.00   1.00    6.50    --  111.00  38.00 -30.00   38
 89  \w    132.00 165.00   1.00    6.50    --  111.00  38.00 -90.00   33
 90  \w     86.00 112.00   1.00    6.50    --  111.00  73.00 -35.25   26
 91  \w     92.00 117.00   1.00    6.50    --  111.00  64.00 120.00   25
 92  \w     49.00 101.00   1.00    6.50    --  111.00 -92.00 120.00   52
 93  \w     86.00 112.00   1.00    6.50    --  111.00  25.00-150.00   26
 94  \w     87.00 126.00   1.00    6.50    --  111.00  25.00  30.00   39
 95  \w    144.00 174.00   1.00    6.50    --  111.00  64.00 -90.00   30
 96  \w     91.00 117.00   1.00    6.50    --  111.00  64.00-150.00   26
 97  \w     91.00 124.00   1.00    6.50    --  111.00  64.00 -90.00   33
 98  \w     84.00 109.00   1.00    6.50    --  111.00-111.00  90.00   25
 99  \w    143.00 170.00   1.00    6.50    --  111.00  38.00-150.00   27
100  \w     92.00 119.00   1.00    6.50    --  111.00  38.00 120.00   27
101  \w     43.00  80.00   1.00    6.50    --  111.00-111.00  90.00   37
102  \w    126.00 174.00   1.00    6.50    --  111.00  50.00 -60.00   48
103  \w     61.00 106.00   1.00    6.50    --  111.00-111.00 -60.00   45
104  \w    145.00 171.00   1.00    6.50    --  111.00  25.00 150.00   26
105  \w    136.00 174.00   1.00    6.50    --  111.00  38.00   0.00   38
106  \w     94.00 121.00   1.00    6.50    --  111.00  50.00 -60.00   27
107  \w     86.00 114.00   1.00    6.50    --  111.00  25.00 150.00   28
108  \w    130.00 176.00   1.00    6.50    --  111.00  64.00 150.00   46
109  \w     57.00 107.00   1.00    6.50    --  111.00-111.00-150.00   50
110  \w    110.00 175.00   1.00    6.50    --  111.00 111.00  90.00   65
111  \w     42.00 109.00   1.00    6.50    --  111.00-111.00  30.00   67
112  \w     68.00  97.00   1.00    6.50    --  111.00 178.00-120.00   29
113  \w    102.00 128.00   1.00    6.50    --  111.00 178.00-120.00   26
114  \w     92.00 134.00   1.00    6.50    --  111.00  38.00  90.00   42
115  \w     42.00  75.00   1.00    6.50    --  111.00 -38.00-180.00   33
116  \w     87.00 129.00   1.00    6.50    --  111.00 -38.00-180.00   42
117  \w     86.00 136.00   1.00    6.50    --  111.00  25.00-180.00   50
118  \w     91.00 117.00   1.00    6.50    --  111.00  64.00 150.00   26
119  \w     58.00 105.00   1.00    6.50    --  111.00-111.00 -30.00   47
120  \w     55.00  90.00   1.00    6.50    --  111.00 -50.00 -90.00   35
121  \w     86.00 178.00   1.00    6.50    --  111.00  25.00-120.00   92
122  \w     51.00  77.00   1.00    6.50    --  111.00 -50.00 -30.00   26
123  \w     79.00 123.00   1.00    6.50    --  111.00 -50.00 -30.00   44
124  \w     94.00 120.00   1.00    6.50    --  111.00  50.00  30.00   26
125  \w     57.00  83.00   1.00    6.50    --  111.00-152.00-125.00   26
126  \w     96.00 121.00   1.00    6.50    --  111.00 -50.00 150.00   25
127  \w     56.00  84.00   1.00    6.50    --  111.00 -50.00 150.00   28
128  \w     91.00 117.00   1.00    6.50    --  111.00  64.00 -60.00   26
129  \w    138.00 165.00   1.00    6.50    --  111.00  64.00-120.00   27
130  \w    130.00 157.00   1.00    6.50    --  111.00  38.00  60.00   27
131  \w     87.00 131.00   1.00    6.50    --  111.00-152.00-125.00   44
132  \w     43.00 115.00   1.00    6.50    --  111.00 -38.00  60.00   72
133  \w    124.00 171.00   1.00    6.50    --  111.00  63.00   5.26   47
;
_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      -0.0590140000
_diffrn_orient_matrix_UB_12      -0.0573392000
_diffrn_orient_matrix_UB_13      0.0217993000
_diffrn_orient_matrix_UB_21      -0.0196761000
_diffrn_orient_matrix_UB_22      -0.0127057000
_diffrn_orient_matrix_UB_23      0.0857615000
_diffrn_orient_matrix_UB_31      -0.0780014000
_diffrn_orient_matrix_UB_32      0.0731924000
_diffrn_orient_matrix_UB_33      -0.0095053000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            113845
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         4.289
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79102
_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    1.640
_exptl_crystal_description       block
_exptl_crystal_F_000             2532
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.066
_refine_diff_density_max         3.205
_refine_diff_density_min         -2.504
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1353
_refine_ls_number_reflns         18307
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0458P)^2^+14.6030P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0954
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16740
_reflns_number_total             18307
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02537f2.cif
_cod_data_source_block           Compound_3a
_cod_original_formula_sum        'C45.50 H41.50 B2 Cl4.50 Mo N12 O4 W'
_cod_database_code               7708367
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C45 H41 B2 Cl3 Mo N12 O4 W'
_chemical_oxdiff_usercomment     c/h
_reflns_odcompleteness_completeness 98.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C86-Cl1 \\sim C86-Cl2 \\sim C86-Cl3 \\sim C86-Cl1A \\sim C86-Cl2A \\sim
C86-Cl3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C86 \\sim Cl1 \\sim Cl2 \\sim Cl3 \\sim Cl1A \\sim Cl2A \\sim Cl3A: within 2A
with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 Sof(H86A)=Sof(Cl2A)=Sof(Cl1A)=Sof(Cl3A)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl2)=Sof(Cl1)=Sof(H86)=FVAR(1)
 Fixed Sof: Cl9(0.5) Cl8(0.5) Cl7(0.5) C85(0.5) H85(0.5) Cl10(0.5) Cl13(0.5)
 Cl11(0.5) C99(0.5)
5.a Ternary CH refined with riding coordinates:
 C87(H87), C86(H86), C86(H86A), C85(H85)
5.b Aromatic/amide H refined with riding coordinates:
 C63(H63), C27(H27), C26(H26), C62(H62), C49(H49), C6(H6), C13(H13), C66(H66),
 C25(H25), C9(H9), C19(H19), C65(H65), C55(H55), C20(H20), C53(H53), C64(H64),
 C77(H77), C46(H46), C16(H16), C21(H21), C14(H14), C30(H30), C40(H40), C8(H8),
 C72(H72), C35(H35), C61(H61), C48(H48), C47(H47), C7(H7), C82(H82), C15(H15),
 C90(H90), C54(H54), C68(H68), C69(H69), C67(H67), C24(H24), C22(H22), C23(H23)
5.c Idealised Me refined as rotating group:
 C80(H80A,H80B,H80C), C38(H38A,H38B,H38C), C70(H70A,H70B,H70C), C28(H28A,H28B,
 H28C), C42(H42A,H42B,H42C), C75(H75A,H75B,H75C), C74(H74A,H74B,H74C), C33(H33A,
 H33B,H33C), C79(H79A,H79B,H79C), C37(H37A,H37B,H37C), C84(H84A,H84B,H84C),
 C32(H32A,H32B,H32C)
;
_shelx_res_checksum              14190
_shelx_hkl_checksum              18591
_ins_header
;
TITL BF141A_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  17.011695  18.790171  19.961342  63.6325  68.5651  69.6860
ZERR    4.00   0.000163   0.000214   0.000236   0.0012   0.0010   0.0010
LATT  1
SFAC C H B N O Cl Mo W
UNIT 180.00 164.00 8.00 48.00 16.00 12.00 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 1.299
_oxdiff_exptl_absorpt_empirical_full_min 0.788