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_7700964
_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 H28 Si2'
_chemical_formula_sum            'C34 H28 Si2'
_chemical_formula_weight         492.74
_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   mixed
_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                 93.3830(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.91870(10)
_cell_length_b                   12.66180(10)
_cell_length_c                   17.4771(2)
_cell_measurement_reflns_used    23364
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      74.2980
_cell_measurement_theta_min      4.3070
_cell_volume                     2632.91(4)
_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      99.9(5)
_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     25.00 175.00   0.50    0.25    --  102.39   0.00  30.00  300
  2  \w    121.00 174.00   0.50    0.25    --  102.39 111.00 120.00  106
  3  \w     73.00 129.00   0.50    0.25    --  102.39  15.00-120.00  112
  4  \w    144.00 177.00   0.50    0.25    --  102.39  15.00-120.00   66
  5  \w    113.00 176.00   0.50    0.25    --  102.39 111.00-180.00  126
  6  \w     81.00 134.00   0.50    0.25    --  102.39  61.00-120.00  106
  7  \w      2.00  29.00   0.50    0.10    --  -47.48  38.00  60.00   54
  8  \w    -71.00  28.00   0.50    0.10    --  -47.48  77.00 120.00  198
  9  \w    -61.00 -32.00   0.50    0.25    --  -90.25  77.00   0.00   58
 10  \w   -106.00 -59.00   0.50    0.25    --  -90.25  30.00-180.00   94
 11  \w     86.00 112.00   0.50    0.25    --  102.39-111.00 120.00   52
 12  \w     41.00  70.00   0.50    0.25    --  102.39-111.00 120.00   58
 13  \w     25.00 101.00   0.50    0.25    --  102.39 -95.00  60.00  152
 14  \w     49.00  92.00   0.50    0.25    --  102.39 -95.00  90.00   86
 15  \w     24.00 104.00   0.50    0.25    --  102.39 -95.00 150.00  160
 16  \w     41.00 115.00   0.50    0.25    --  102.39-111.00 -30.00  148
 17  \w     23.00 107.00   0.50    0.25    --  102.39 -95.00 -30.00  168
 18  \w     79.00 104.00   0.50    0.25    --  102.39 -95.00-150.00   50
 19  \w    -60.00 -32.00   0.50    0.25    --  -90.25  61.00 -90.00   56
 20  \w    -50.00 -13.00   0.50    0.25    --  -90.25  30.00-180.00   74
 21  \w   -116.00 -89.00   0.50    0.25    --  -90.25  77.00   0.00   54
 22  \w    -99.00 -30.00   0.50    0.10    --  -47.48 -57.00   0.00  138
 23  \w   -123.00 -21.00   0.50    0.10    --  -47.48 -77.00 -60.00  204
 24  \w     35.00 116.00   0.50    0.25    --  102.39 -77.00 150.00  162
 25  \w     54.00 122.00   0.50    0.25    --  102.39 -61.00 150.00  136
 26  \w     24.00  53.00   0.50    0.25    --  102.39 -30.00-120.00   58
 27  \w   -164.00-128.00   0.50    0.25    --  -90.25 -45.00 -30.00   72
 28  \w   -116.00 -77.00   0.50    0.25    --  -90.25 -45.00 -30.00   78
 29  \w   -120.00 -93.00   0.50    0.10    --  -47.48-125.00  90.00   54
 30  \w   -109.00 -84.00   0.50    0.10    --  -47.48-125.00 150.00   50
 31  \w   -121.00 -95.00   0.50    0.10    --  -47.48-125.00 -60.00   52
 32  \w   -110.00 -70.00   0.50    0.10    --  -47.48-125.00-150.00   80
;
_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      0.0398887000
_diffrn_orient_matrix_UB_12      0.1134550000
_diffrn_orient_matrix_UB_13      -0.0154236000
_diffrn_orient_matrix_UB_21      0.0880591000
_diffrn_orient_matrix_UB_22      -0.0089634000
_diffrn_orient_matrix_UB_23      0.0678659000
_diffrn_orient_matrix_UB_31      0.0860925000
_diffrn_orient_matrix_UB_32      -0.0432315000
_diffrn_orient_matrix_UB_33      -0.0543027000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28300
_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         5.599
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.370
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85168
_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    1.243
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.043
_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     333
_refine_ls_number_reflns         4763
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0385P)^2^+1.3190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4501
_reflns_number_total             4763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03058a2.cif
_cod_data_source_block           18a
_cod_depositor_comments
'Adding full bibliography for 7700964--7700969.cif.'
_cod_database_code               7700964
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C34H28Si2
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.668
_reflns_odcompleteness_completeness 99.98
_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)
;
_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 1.216
_oxdiff_exptl_absorpt_empirical_full_min 0.793