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_7700966
_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 O0.1 Si2'
_chemical_formula_sum            'C14 H18 O0.1 Si2'
_chemical_formula_weight         243.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-06-28
_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                90
_cell_angle_beta                 94.0488(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.35819(19)
_cell_length_b                   8.27537(16)
_cell_length_c                   19.9683(4)
_cell_measurement_reflns_used    7409
_cell_measurement_temperature    99.97(13)
_cell_measurement_theta_max      74.0190
_cell_measurement_theta_min      5.6320
_cell_volume                     1377.70(5)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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    -28.00  75.00   0.50    0.33    --   47.48 -79.00-119.00  206
  2  \w     22.00  65.00   0.50    0.33    --   47.48  79.00   4.00   86
  3  \w     70.00  98.00   0.50    0.33    --   47.48  79.00   4.00   56
  4  \w    -85.00 -14.00   0.50    1.30    --  -90.25  79.00   4.00  142
  5  \w     29.00  97.00   0.50    1.30    --  101.53 -79.00-119.00  136
  6  \w    125.00 155.00   0.50    1.30    --  101.53  79.00   4.00   60
  7  \w   -123.00 -72.00   0.50    0.33    --  -47.48-125.00 -60.00  102
  8  \w    -27.00   1.00   0.50    0.33    --  -47.48  79.00   4.00   56
  9  \w   -120.00 -92.00   0.50    0.33    --  -47.48-125.00  90.00   56
 10  \w   -116.00 -79.00   0.50    0.33    --  -47.48-125.00 150.00   74
 11  \w   -118.00 -44.00   0.50    0.33    --  -47.48 -57.00-180.00  148
 12  \w   -124.00 -99.00   0.50    0.33    --  -47.48-125.00-180.00   50
 13  \w   -111.00 -68.00   0.50    1.30    --  -90.25 -61.00 150.00   86
 14  \w   -124.00 -82.00   0.50    1.30    --  -90.25 -94.00-180.00   84
 15  \w   -161.00-119.00   0.50    1.30    --  -90.25 -61.00 150.00   84
 16  \w   -168.00 -94.00   0.50    1.30    --  -90.25 -94.00 -90.00  148
 17  \w   -158.00 -79.00   0.50    1.30    --  -90.25-111.00 -30.00  158
 18  \w     77.00 107.00   0.50    1.30    --  101.53  77.00  60.00   60
 19  \w    148.00 174.00   0.50    1.30    --  101.53  77.00 -60.00   52
 20  \w     81.00 175.00   0.50    1.30    --  101.53  61.00  30.00  188
 21  \w     22.00  89.00   0.50    1.30    --  101.53 -94.00-180.00  134
 22  \w     79.00 141.00   0.50    1.30    --  101.53  77.00 -60.00  124
 23  \w     84.00 110.00   0.50    1.30    --  101.53  45.00  60.00   52
 24  \w     43.00  90.00   0.50    1.30    --  101.53 -45.00 -90.00   94
 25  \w     81.00 175.00   0.50    1.30    --  101.53  61.00 120.00  188
 26  \w    123.00 155.00   0.50    1.30    --  101.53  30.00 -60.00   64
 27  \w     60.00 149.00   0.50    1.30    --  101.53 178.00 150.00  178
 28  \w    119.00 150.00   0.50    1.30    --  101.53  45.00  60.00   62
 29  \w     25.00 111.00   0.50    1.30    --  101.53-111.00 -30.00  172
 30  \w    123.00 167.00   0.50    1.30    --  101.53  77.00  60.00   88
 31  \w     83.00 117.00   0.50    1.30    --  101.53  30.00 -60.00   68
;
_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      0.0048244000
_diffrn_orient_matrix_UB_12      -0.0843973000
_diffrn_orient_matrix_UB_13      -0.0685413000
_diffrn_orient_matrix_UB_21      -0.1061578000
_diffrn_orient_matrix_UB_22      0.1344979000
_diffrn_orient_matrix_UB_23      -0.0328376000
_diffrn_orient_matrix_UB_31      0.1511809000
_diffrn_orient_matrix_UB_32      0.0972704000
_diffrn_orient_matrix_UB_33      -0.0142041000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14649
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.196
_diffrn_reflns_theta_min         4.440
_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  0.92036
_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    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             523
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2767
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0331P)^2^+0.5914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2526
_reflns_number_total             2767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03058a2.cif
_cod_data_source_block           cpd_169_split
_cod_depositor_comments
'Adding full bibliography for 7700964--7700969.cif.'
_cod_original_formula_sum        'C14 H18 O0.10 Si2'
_cod_database_code               7700966
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C14H18Si2
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.679
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1A-O1 = Si2A-O1
 1.64 with sigma of 0.02
 Si1A-C2A = Si1A-C1A
 1.89 with sigma of 0.02
 Si2A-C4A = Si2A-C3A
 1.89 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Si1) = Uanis(Si1A)
Uanis(Si2) = Uanis(Si2A)
Uanis(C4) = Uanis(C4A)
Uanis(C3) = Uanis(C3A)
Uanis(C2) = Uanis(C2A)
Uanis(C1) = Uanis(C1A)
4. Others
 Sof(Si1)=Sof(Si2)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=
 Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(H4C)=1-FVAR(1)
 Sof(Si1A)=Sof(Si2A)=Sof(O1)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C1A(H1AA,
 H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC)
;
_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 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.859