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_7700965
_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         'C34.1 H26 O0.1 Si2'
_chemical_formula_sum            'C34.1 H26 O0.1 Si2'
_chemical_formula_weight         493.60
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                 106.959(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6489(3)
_cell_length_b                   8.81950(10)
_cell_length_c                   19.3548(3)
_cell_measurement_reflns_used    14234
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      74.3340
_cell_measurement_theta_min      2.9590
_cell_volume                     2555.10(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (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      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_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    -34.00  14.00   0.50    0.10    --  -47.48  44.00-107.00   96
  2  \w    -68.00 -26.00   0.50    0.10    --  -47.48 -38.00 -60.00   84
  3  \w   -100.00 -75.00   0.50    0.10    --  -47.48 -44.00 101.00   50
  4  \w    -66.00 -39.00   0.50    0.10    --  -47.48 -44.00 101.00   54
  5  \w   -111.00 -26.00   0.50    0.42    --  -90.25  61.00   0.00  170
  6  \w    -89.00 -36.00   0.50    0.42    --  -90.25 111.00   0.00  106
  7  \w   -162.00 -70.00   0.50    0.42    --  -90.25 -44.00 101.00  184
  8  \w   -124.00 -73.00   0.50    0.10    --  -47.48-125.00  60.00  102
  9  \w   -124.00 -71.00   0.50    0.10    --  -47.48-125.00  30.00  106
 10  \w   -123.00 -71.00   0.50    0.10    --  -47.48-125.00-180.00  104
 11  \w     32.00 114.00   0.50    0.10    --   47.48  57.00 -60.00  164
 12  \w    115.00 141.00   0.50    0.42    --  102.39  44.00-107.00   52
 13  \w     90.00 178.00   0.50    0.42    --  102.39  45.00 -30.00  176
 14  \w    148.00 173.00   0.50    0.42    --  102.39 111.00-120.00   50
 15  \w     83.00 178.00   0.50    0.42    --  102.39  45.00   0.00  190
 16  \w     57.00  83.00   0.50    0.42    --  102.39 -44.00 101.00   52
 17  \w     36.00 105.00   0.50    0.42    --  102.39 -61.00  60.00  138
 18  \w     51.00 108.00   0.50    0.42    --  102.39 -95.00 -90.00  114
 19  \w     27.00 120.00   0.50    0.42    --  102.39 -45.00-180.00  186
 20  \w     52.00  77.00   0.50    0.10    --   47.48  44.00-107.00   50
 21  \w     31.00  56.00   0.50    0.42    --  102.39 -95.00-150.00   50
 22  \w     24.00  84.00   0.50    0.42    --  102.39 -95.00  30.00  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      -0.0819649000
_diffrn_orient_matrix_UB_12      0.0955303000
_diffrn_orient_matrix_UB_13      0.0011745000
_diffrn_orient_matrix_UB_21      0.0301361000
_diffrn_orient_matrix_UB_22      -0.0042991000
_diffrn_orient_matrix_UB_23      0.0831897000
_diffrn_orient_matrix_UB_31      0.0544904000
_diffrn_orient_matrix_UB_32      0.1461450000
_diffrn_orient_matrix_UB_33      0.0015917000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19186
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.735
_diffrn_reflns_theta_min         5.556
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.417
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       needle
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.00046(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         4633
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0469P)^2^+1.1302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4237
_reflns_number_total             4633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03058a2.cif
_cod_data_source_block           19b_split
_cod_depositor_comments
'Adding full bibliography for 7700964--7700969.cif.'
_cod_original_formula_sum        'C34.10 H26 O0.10 Si2'
_cod_database_code               7700965
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C34H26Si2
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.826
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.62
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All Si(O) groups
2. Restrained distances
 Si1A-O1 = Si2A-O1
 1.65 with sigma of 0.02
 Si1A-C6A = Si1A-C7A = Si2A-C23A = Si2A-C29A
 1.88 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(Si1) = Uanis(Si1A)
Uanis(Si2) = Uanis(Si2A)
Uanis(C1) = Uanis(C1A)
Uanis(C2) = Uanis(C2A)
Uanis(C3) = Uanis(C3A)
Uanis(C4) = Uanis(C4A)
Uanis(C5) = Uanis(C5A)
Uanis(C6) = Uanis(C6A)
Uanis(C7) = Uanis(C7A)
Uanis(C8) = Uanis(C8A)
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
Uanis(C11) = Uanis(C11A)
Uanis(C12) = Uanis(C12A)
Uanis(C23) = Uanis(C23A)
Uanis(C24) = Uanis(C24A)
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
Uanis(C27) = Uanis(C27A)
Uanis(C28) = Uanis(C28A)
Uanis(C29) = Uanis(C29A)
Uanis(C30) = Uanis(C30A)
Uanis(C31) = Uanis(C31A)
Uanis(C32) = Uanis(C32A)
Uanis(C33) = Uanis(C33A)
Uanis(C34) = Uanis(C34A)
4. Others
 Sof(Si1)=Sof(Si2)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C7)=Sof(C8)=Sof(H8)=Sof(H9)=Sof(C10)=
 Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C23)=Sof(C24)=Sof(H24)=
 Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=
 Sof(C29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=
 Sof(H33)=Sof(C34)=Sof(H34)=1-FVAR(1)
 Sof(Si1A)=Sof(Si2A)=Sof(O1)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=
 Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C7A)=Sof(C8A)=
 Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=
 Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(C30A)=
 Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=
 Sof(C34A)=Sof(H34A)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C1A(H1A),
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C8A(H8A), C9A(H9A), C10A(H10A),
 C11A(H11A), C12A(H12A), C24A(H24A), C25A(H25A), C26A(H26A), C27A(H27A),
 C28A(H28A), C30A(H30A), C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A), C1(H1),
  C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34)
5.b Fitted hexagon refined as free rotating group:
 C1A(C2A,C3A,C4A,C5A,C6A), C7A(C8A,C9A,C10A,C11A,C12A), C23A(C24A,C25A,C26A,
 C27A,C28A), C29A(C30A,C31A,C32A,C33A,C34A)
;
_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 1.128
_oxdiff_exptl_absorpt_empirical_full_min 0.896