Synthesis, characterisation and electronic properties of naphthalene bridged disilanes.
Rabanzo-Castillo, Kristel M; Hanif, Muhammad; Söhnel, Tilo; Leitao, Erin M.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13971–13980; doi:10.1039/c9dt03058a

data_7700968
_publ_section_title
;
 Synthesis, characterisation and electronic properties of naphthalene
 bridged disilanes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13971
_journal_page_last               13980
_journal_paper_doi               10.1039/c9dt03058a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C14 H18 O Si2'
_chemical_formula_sum            'C14 H18 O Si2'
_chemical_formula_weight         258.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-28 deposited with the CCDC.    2019-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                116.7870(10)
_cell_angle_beta                 96.6352(9)
_cell_angle_gamma                112.9004(10)
_cell_formula_units_Z            4
_cell_length_a                   12.20007(13)
_cell_length_b                   12.30177(13)
_cell_length_c                   12.38995(13)
_cell_measurement_reflns_used    31036
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      74.0630
_cell_measurement_theta_min      4.1770
_cell_volume                     1430.24(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -88.00  -6.00   0.50    0.12    --  -47.48 120.00 -81.00  164
  2  \w   -111.00 -29.00   0.50    0.12    --  -47.48 156.00  74.00  164
  3  \w   -123.00 -98.00   0.50    0.12    --  -47.48-120.00-165.00   50
  4  \w    -80.00 -55.00   0.50    0.12    --  -47.48-156.00  38.00   50
  5  \w     58.00  83.00   0.50    0.12    --   47.48-156.00  38.00   50
  6  \w     35.00  63.00   0.50    0.12    --   47.48-120.00-165.00   56
  7  \w     73.00  98.00   0.50    0.12    --   47.48 156.00  74.00   50
  8  \w    -74.00 -49.00   0.50    0.47    --  -90.25 120.00 -81.00   50
  9  \w    -93.00 -68.00   0.50    0.47    --  -90.25 156.00  74.00   50
 10  \w   -145.00 -99.00   0.50    0.47    --  -90.25-156.00  38.00   92
 11  \w   -145.00-120.00   0.50    0.47    --  -90.25-120.00-165.00   50
 12  \w     82.00 118.00   0.50    0.47    --  101.53 156.00  74.00   72
 13  \w     92.00 117.00   0.50    0.47    --  101.53-156.00  38.00   50
 14  \w     47.00 114.00   0.50    0.47    --  101.53-120.00-165.00  134
 15  \w     95.00 129.00   0.50    0.47    --  101.53 120.00 -81.00   68
 16  \w    -56.00 -31.00   0.50    0.12    --   14.00 156.00 -61.99   50
 17  \w    -12.00  24.00   0.50    0.12    --   22.00  95.00 173.72   72
 18  \w     -9.00  16.00   0.50    0.12    --   30.00 102.00 -46.74   50
 19  \w      5.00  31.00   0.50    0.12    --   42.00  98.00 -32.02   52
 20  \w      6.00  31.00   0.50    0.12    --   42.00  97.00 112.10   50
 21  \w    -60.00 -24.00   0.50    0.12    --  -47.48 -19.00-180.00   72
 22  \w    -89.00 -58.00   0.50    0.12    --  -47.48 -38.00 120.00   62
 23  \w    -81.00 -25.00   0.50    0.12    --  -47.48 -19.00 -90.00  112
 24  \w   -123.00 -86.00   0.50    0.12    --  -47.48 -19.00 -90.00   74
 25  \w   -107.00 -80.00   0.50    0.12    --  -47.48 -19.00-180.00   54
 26  \w    -56.00 -28.00   0.50    0.12    --  -47.48 -38.00 120.00   56
 27  \w     35.00  61.00   0.50    0.12    --   47.48-125.00  60.00   52
 28  \w     17.00  42.00   0.50    0.12    --   50.00  90.00 -62.78   50
 29  \w     16.00  41.00   0.50    0.12    --   50.00  92.00-108.08   50
 30  \w     16.00  41.00   0.50    0.12    --   50.00  92.00   4.30   50
 31  \w     17.00  42.00   0.50    0.12    --   50.00  90.00  61.73   50
 32  \w     26.00  57.00   0.50    0.12    --   54.00  82.00-145.45   62
 33  \w    -74.00 -31.00   0.50    0.12    --  -58.00 -80.00  89.23   86
 34  \w     29.00  55.00   0.50    0.12    --   58.00  81.00-178.30   52
 35  \w     29.00  55.00   0.50    0.12    --   58.00  83.00  -8.88   52
 36  \w     34.00  66.00   0.50    0.12    --   62.00  81.00  23.82   64
 37  \w     33.00  59.00   0.50    0.12    --   62.00  81.00 133.38   52
 38  \w     33.00  59.00   0.50    0.12    --   62.00  81.00   6.29   52
 39  \w     36.00  68.00   0.50    0.12    --   62.00  80.00  58.31   64
 40  \w    -74.00 -41.00   0.50    0.12    --  -66.00 -71.00-112.33   66
 41  \w     37.00  63.00   0.50    0.12    --   66.00  83.00-114.56   52
 42  \w     39.00  66.00   0.50    0.12    --   66.00  77.00 121.41   54
 43  \w     43.00  84.00   0.50    0.12    --   70.00  80.00  77.78   82
 44  \w    -73.00 -47.00   0.50    0.47    --  -70.00 -71.00 -54.83   52
 45  \w     42.00  70.00   0.50    0.12    --   70.00  80.00-153.07   56
 46  \w    -69.00 -43.00   0.50    0.47    --  -70.00 -76.00-141.21   52
 47  \w     41.00  67.00   0.50    0.12    --   70.00  82.00 -71.32   52
 48  \w    -75.00 -49.00   0.50    0.47    --  -74.00 -71.00 178.55   52
 49  \w     46.00  80.00   0.50    0.12    --   74.00  79.00 -59.96   68
 50  \w   -100.00 -48.00   0.50    0.47    --  -74.00 -74.00  -1.23  104
 51  \w    -77.00 -51.00   0.50    0.47    --  -78.00 -76.00 143.51   52
 52  \w    -78.00 -52.00   0.50    0.47    --  -78.00 -75.00 156.16   52
 53  \w    -82.00 -51.00   0.50    0.47    --  -78.00 -78.00 130.04   62
 54  \w    -88.00 -54.00   0.50    0.47    --  -78.00 -69.00-148.39   68
 55  \w    -79.00 -54.00   0.50    0.47    --  -78.00 -70.00-161.69   50
 56  \w   -144.00-118.00   0.50    0.47    --  -78.00 -78.00 130.04   52
 57  \w    -88.00 -55.00   0.50    0.47    --  -82.00 -76.00  41.89   66
 58  \w    -92.00 -54.00   0.50    0.47    --  -82.00 -78.00 117.42   76
 59  \w    -87.00 -61.00   0.50    0.47    --  -82.00 -68.00 168.54   52
 60  \w    -85.00 -59.00   0.50    0.47    --  -86.00 -76.00 143.08   52
 61  \w    -87.00 -61.00   0.50    0.47    --  -86.00 -71.00 -11.81   52
 62  \w    -99.00 -63.00   0.50    0.47    --  -90.00 -76.00 -83.33   72
 63  \w    -91.00 -64.00   0.50    0.47    --  -90.25 -76.00  55.37   54
 64  \w   -107.00 -65.00   0.50    0.47    --  -90.25 -75.00 160.71   84
 65  \w   -166.00-117.00   0.50    0.47    --  -90.25 -75.00 160.71   98
 66  \w    -95.00 -67.00   0.50    0.47    --  -90.25 -79.00 118.60   56
 67  \w   -113.00 -64.00   0.50    0.47    --  -90.25 -77.00 -90.00   98
 68  \w    -86.00 -45.00   0.50    0.47    --  -90.25 111.00 -90.00   82
 69  \w   -154.00-117.00   0.50    0.47    --  -90.25 -77.00 -90.00   74
 70  \w   -166.00-113.00   0.50    0.47    --  -90.25 -79.00 118.60  106
 71  \w    -88.00 -63.00   0.50    0.47    --  -90.25 -77.00 -60.00   50
 72  \w    -88.00 -63.00   0.50    0.47    --  -90.25 -77.00 -30.00   50
 73  \w   -166.00-113.00   0.50    0.47    --  -90.25 -76.00  55.37  106
 74  \w   -150.00-103.00   0.50    0.47    --  -90.25 -77.00 -60.00   94
 75  \w    -90.00 -65.00   0.50    0.47    --  -90.25 -72.00 -43.49   50
 76  \w    -89.00 -63.00   0.50    0.47    --  -90.25 -77.00-120.00   52
 77  \w   -164.00-109.00   0.50    0.47    --  -90.25 -77.00-120.00  110
 78  \w   -161.00-116.00   0.50    0.47    --  -90.25 -72.00 -43.49   90
 79  \w   -160.00 -67.00   0.50    0.47    --  -90.25 -77.00-108.62  186
 80  \w    -93.00 -68.00   0.50    0.47    --  -90.25 -65.00-149.89   50
 81  \w    -91.00 -65.00   0.50    0.47    --  -90.25 -77.00-180.00   52
 82  \w   -162.00-137.00   0.50    0.47    --  -90.25 -77.00  38.88   50
 83  \w   -126.00 -68.00   0.50    0.47    --  -90.25 -72.00   6.90  116
 84  \w   -110.00 -63.00   0.50    0.47    --  -90.25 -77.00  38.88   94
 85  \w   -156.00 -65.00   0.50    0.47    --  -90.25 -75.00  72.78  182
 86  \w   -115.00 -63.00   0.50    0.47    --  -90.25 -77.00  30.00  104
 87  \w   -114.00 -64.00   0.50    0.47    --  -90.25 -76.00 142.57  100
 88  \w    -88.00 -63.00   0.50    0.47    --  -90.25 -77.00-150.00   50
 89  \w    -89.00 -64.00   0.50    0.47    --  -90.25 -77.00 120.00   50
 90  \w   -148.00-114.00   0.50    0.47    --  -90.25 -77.00 120.00   68
 91  \w   -164.00-104.00   0.50    0.47    --  -90.25 -77.00-150.00  120
 92  \w   -153.00-126.00   0.50    0.47    --  -90.25 -77.00  30.00   54
 93  \w   -148.00-107.00   0.50    0.47    --  -90.25 -71.00-167.94   82
 94  \w    -92.00 -61.00   0.50    0.47    --  -90.25 -81.00 -63.21   62
 95  \w   -158.00 -70.00   0.50    0.47    --  -90.25 -61.00 -41.67  176
 96  \w   -102.00 -65.00   0.50    0.47    --  -90.25 -76.00  -6.76   74
 97  \w   -165.00-115.00   0.50    0.47    --  -90.25 -76.00  -6.76  100
 98  \w   -116.00 -68.00   0.50    0.47    --  -90.25 -66.00 176.88   96
 99  \w   -144.00 -63.00   0.50    0.47    --  -90.25 -77.00  90.00  162
100  \w   -166.00-123.00   0.50    0.47    --  -90.25 -81.00 -63.21   86
101  \w   -166.00-121.00   0.50    0.47    --  -90.25 -76.00 142.57   90
102  \w     22.00 108.00   0.50    0.47    --  101.53 -94.00 150.00  172
103  \w     32.00 128.00   0.50    0.47    --  101.53 -77.00   0.00  192
104  \w     86.00 164.00   0.50    0.47    --  101.53  61.00 120.00  156
105  \w     60.00 121.00   0.50    0.47    --  101.53 -61.00-180.00  122
106  \w     73.00 107.00   0.50    0.47    --  101.53 -94.00 -90.00   68
107  \w     78.00 109.00   0.50    0.47    --  101.53  77.00 -60.00   62
108  \w     90.00 133.00   0.50    0.47    --  101.53  77.00-150.00   86
109  \w     27.00  67.00   0.50    0.47    --  101.53 -94.00 -90.00   80
110  \w     78.00 104.00   0.50    0.47    --  101.53 -94.00-120.00   52
111  \w     24.00  58.00   0.50    0.47    --  101.53 -94.00-120.00   68
112  \w     54.00 109.00   0.50    0.47    --  101.53 -94.00   0.00  110
113  \w     61.00 121.00   0.50    0.47    --  101.53 178.00 -90.00  120
114  \w     62.00 122.00   0.50    0.47    --  101.53 -61.00   0.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0808286000
_diffrn_orient_matrix_UB_12      -0.0717525000
_diffrn_orient_matrix_UB_13      -0.0356565000
_diffrn_orient_matrix_UB_21      0.1209120000
_diffrn_orient_matrix_UB_22      0.1448775000
_diffrn_orient_matrix_UB_23      0.0686982000
_diffrn_orient_matrix_UB_31      0.0180524000
_diffrn_orient_matrix_UB_32      0.0041999000
_diffrn_orient_matrix_UB_33      0.1272222000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            43511
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.228
_diffrn_reflns_theta_min         6.544
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.102
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         5232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0358P)^2^+0.5013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4811
_reflns_number_total             5232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03058a2.cif
_cod_data_source_block           3me
_cod_depositor_comments
'Adding full bibliography for 7700964--7700969.cif.'
_cod_original_cell_volume        1430.24(3)
_cod_database_code               7700968
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C28H38O2Si4
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.704
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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:
 C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C20(H20), C21(H21),
 C22(H22), C24(H24), C25(H25), C26(H26)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C15(H15A,
 H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_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 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.902