The photophysical properties of naphthalene bridged disilanes
Kumar, Vipin B.; Fleming, Cassandra L.; Murali, Sai Shruthi; Hume, Paul A.; Davis, Nathaniel J. L. K.; Söhnel, Tilo; Leitao, Erin M.; RSC Advances 11 (2021) 21343–21350; doi:10.1039/D1RA02961D

data_7243066
_publ_section_title
;
 The photophysical properties of naphthalene bridged disilanes
;
_journal_issue                   35
_journal_name_full               'RSC Advances'
_journal_page_first              21343
_journal_page_last               21350
_journal_paper_doi               10.1039/D1RA02961D
_journal_volume                  11
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H22 Si2'
_chemical_formula_sum            'C24 H22 Si2'
_chemical_formula_weight         366.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-02-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-04 deposited with the CCDC.	2021-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.7979(2)
_cell_length_b                   36.7369(6)
_cell_length_c                   14.1416(2)
_cell_measurement_reflns_used    10911
_cell_measurement_temperature    100.7(7)
_cell_measurement_theta_max      74.1310
_cell_measurement_theta_min      3.3590
_cell_volume                     4051.15(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.7(7)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_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     11.00  85.00   0.50    0.60    --   47.48 -99.00-150.00  148
  2  \w     56.00 105.00   0.50    2.50    --  101.53-126.00-158.00   98
  3  \w    103.00 128.00   0.50    2.50    --  101.53 -77.00-180.00   50
  4  \w     86.00 112.00   0.50    2.50    --  101.53 -30.00-120.00   52
  5  \w     35.00  74.00   0.50    0.60    --   47.48-125.00 -60.00   78
  6  \w     22.00  80.00   0.50    2.50    --  101.53 -94.00   0.00  116
  7  \w     26.00 110.00   0.50    2.50    --  101.53 -94.00  60.00  168
  8  \w     28.00 129.00   0.50    2.50    --  101.53 -77.00  60.00  202
  9  \w     29.00  97.00   0.50    2.50    --  101.53 -77.00-180.00  136
 10  \w    124.00 173.00   0.50    2.50    --  101.53 111.00  90.00   98
 11  \w    129.00 158.00   0.50    2.50    --  101.53 111.00 -30.00   58
 12  \w     99.00 178.00   0.50    2.50    --  101.53 111.00 150.00  158
 13  \w    -62.00 -37.00   0.50    2.50    --  -90.25  46.00-140.00   50
 14  \w    -89.00 -64.00   0.50    2.50    --  -90.25  75.00  36.00   50
 15  \w   -168.00 -78.00   0.50    2.50    --  -90.25 -46.00  69.00  180
 16  \w   -122.00 -71.00   0.50    0.60    --  -47.48-125.00   0.00  102
 17  \w   -120.00 -91.00   0.50    0.60    --  -47.48-144.00  33.00   58
 18  \w   -101.00 -74.00   0.50    0.60    --  -47.48-126.00-158.00   54
 19  \w   -107.00 -74.00   0.50    0.60    --  -47.48-125.00-180.00   66
;
_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      0.0991071000
_diffrn_orient_matrix_UB_12      -0.0306456000
_diffrn_orient_matrix_UB_13      0.0504706000
_diffrn_orient_matrix_UB_21      0.1704989000
_diffrn_orient_matrix_UB_22      0.0160684000
_diffrn_orient_matrix_UB_23      -0.0359856000
_diffrn_orient_matrix_UB_31      0.0126337000
_diffrn_orient_matrix_UB_32      0.0236961000
_diffrn_orient_matrix_UB_33      0.0895363000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            26139
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.243
_diffrn_reflns_theta_min         5.744
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 2596 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.036(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0331P)^2^+0.7551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0824
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6498
_reflns_number_total             7418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra02961d2.cif
_cod_data_source_block           vk53
_cod_database_code               7243066
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C24H22Si2
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.924
_reflns_odcompleteness_completeness 99.95
_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:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C26(H26),
  C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34),
 C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C44(H44)
2.b Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C)
;
_shelx_res_checksum              19051
_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 1.210
_oxdiff_exptl_absorpt_empirical_full_min 0.840