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_7700967
_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 H26 O Si2'
_chemical_formula_sum            'C34 H26 O Si2'
_chemical_formula_weight         506.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-21 deposited with the CCDC.    2019-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.6440(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   20.0464(2)
_cell_length_b                   8.79710(10)
_cell_length_c                   44.8873(6)
_cell_measurement_reflns_used    26034
_cell_measurement_temperature    99.9(7)
_cell_measurement_theta_max      74.4770
_cell_measurement_theta_min      3.9330
_cell_volume                     7877.51(16)
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_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    -57.00 -22.00   0.50    0.61    --  -47.48  74.00 -28.00   70
  2  \w    -90.00 -65.00   0.50    2.43    --  -90.25  74.00 -28.00   50
  3  \w   -111.00 -18.00   0.50    2.43    --  -90.25  45.00 -30.00  186
  4  \w    -59.00 -27.00   0.50    0.61    --  -47.48 -57.00-180.00   64
  5  \w    -97.00 -72.00   0.50    0.61    --  -47.48 -74.00-156.00   50
  6  \w     48.00  73.00   0.50    0.61    --   47.48  74.00 -28.00   50
  7  \w     85.00 120.00   0.50    2.43    --  102.39  74.00 -28.00   70
  8  \w    142.00 169.00   0.50    2.43    --  102.39  74.00 -28.00   54
  9  \w    122.00 177.00   0.50    2.43    --  102.39  45.00 -90.00  110
 10  \w    132.00 177.00   0.50    2.43    --  102.39  45.00-120.00   90
 11  \w    128.00 164.00   0.50    2.43    --  102.39 111.00-180.00   72
 12  \w     86.00 114.00   0.50    2.43    --  102.39  45.00-120.00   56
 13  \w     44.00 124.00   0.50    2.43    --  102.39 -61.00-150.00  160
 14  \w     53.00  78.00   0.50    2.43    --  102.39 -74.00-156.00   50
 15  \w     -2.00  23.00   0.50    0.61    --   47.48 -74.00-156.00   50
 16  \w     87.00 172.00   0.50    2.43    --  102.39  30.00  60.00  170
 17  \w    109.00 134.00   0.50    2.43    --  102.39 111.00  90.00   50
 18  \w     33.00  95.00   0.50    0.61    --   47.48-125.00  90.00  124
 19  \w   -113.00 -70.00   0.50    0.61    --  -47.48-125.00  90.00   86
 20  \w   -113.00 -87.00   0.50    0.61    --  -47.48-125.00 120.00   52
 21  \w   -123.00 -98.00   0.50    0.61    --  -47.48-125.00 -90.00   50
 22  \w   -121.00 -90.00   0.50    0.61    --  -47.48 -57.00-180.00   62
 23  \w   -161.00 -68.00   0.50    2.43    --  -90.25 -61.00-180.00  186
 24  \w   -104.00 -22.00   0.50    2.43    --  -90.25  30.00 120.00  164
;
_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      -0.0766865000
_diffrn_orient_matrix_UB_12      -0.0062539000
_diffrn_orient_matrix_UB_13      0.0004258000
_diffrn_orient_matrix_UB_21      -0.0027176000
_diffrn_orient_matrix_UB_22      -0.1427315000
_diffrn_orient_matrix_UB_23      -0.0199735000
_diffrn_orient_matrix_UB_31      0.0085362000
_diffrn_orient_matrix_UB_32      -0.1012719000
_diffrn_orient_matrix_UB_33      0.0281206000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            26277
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.245
_diffrn_reflns_theta_min         5.649
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72585
_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    1.282
_exptl_crystal_description       plate
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         7144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+9.1704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6849
_reflns_number_total             7144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03058a2.cif
_cod_data_source_block           cpd19
_cod_depositor_comments
'Adding full bibliography for 7700964--7700969.cif.'
_cod_database_code               7700967
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C34H26Si2
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.644
_reflns_odcompleteness_completeness 99.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.62
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C1'(H1'), C2'(H2'), C3'(H3'), C4'(H4'), C5'(H5'), C8'(H8'),
  C9'(H9'), C10'(H10'), C11'(H11'), C12'(H12'), C14'(H14'), C15'(H15'),
 C16'(H16')
;
_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 1.498
_oxdiff_exptl_absorpt_empirical_full_min 0.671