Structural and electronic studies of substituted m-terphenyl lithium complexes.
Valentine, Andrew J.; Geer, Ana M.; Taylor, Laurence J.; Teale, Andrew M.; Wood, Katherine E.; Williams, Huw E. L.; Lewis, William; Argent, Stephen P.; McMaster, Jonathan; Kays, Deborah L.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 722–728; doi:10.1039/d0dt03972a

data_7705998
_publ_section_title
;
 Structural and electronic studies of substituted m-terphenyl lithium
 complexes.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              722
_journal_page_last               728
_journal_paper_doi               10.1039/d0dt03972a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C25 H29 I Si'
_chemical_formula_sum            'C25 H29 I Si'
_chemical_formula_weight         484.47
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-06-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.860(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3663(4)
_cell_length_b                   17.8142(9)
_cell_length_c                   20.5558(14)
_cell_measurement_reflns_used    3889
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.3570
_cell_measurement_theta_min      4.9460
_cell_volume                     2314.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9569
_diffrn_measurement_details
;
  1 omega   56.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000    0.0000 34

  2 omega   74.00  128.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -77.0000  -30.0000 54

  3 omega   38.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000   90.0000 52

  4 omega   39.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -45.0000   60.0000 59

  5 omega   36.00  116.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322 -125.0000   30.0000 80

  6 omega   17.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.2215  -99.0000  -30.0000 38

  7 omega  -34.00    6.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -30.0000 40

  8 omega  -48.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   90.0000 80

  9 omega -105.00  -77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000 -120.0000   86.8067 28

 10 omega   70.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3777 -125.0000 -150.0000 28

 11 omega    9.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3777  -99.0000 -180.0000 44

 12 omega  138.00  165.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  125.0000   60.0000 27

 13 omega   49.00   75.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000  -60.0000 26

 14 omega   35.00   76.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -30.0000 -150.0000 41

 15 omega   29.00  106.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      106.1322  -15.0000 -120.0000 77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      0.0409552000
_diffrn_orient_matrix_UB_12      -0.0850241000
_diffrn_orient_matrix_UB_13      -0.0031750000
_diffrn_orient_matrix_UB_21      -0.0826238000
_diffrn_orient_matrix_UB_22      0.0001573000
_diffrn_orient_matrix_UB_23      -0.0735312000
_diffrn_orient_matrix_UB_31      0.2257795000
_diffrn_orient_matrix_UB_32      0.0155478000
_diffrn_orient_matrix_UB_33      -0.0166862000
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9764
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.502
_diffrn_reflns_theta_min         3.293
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.395
_exptl_absorpt_correction_T_max  0.539
_exptl_absorpt_correction_T_min  0.090
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       needle
_exptl_crystal_F_000             984
_exptl_crystal_recrystallization_method 'Recrystallised from diethyl ether'
_exptl_crystal_size_max          0.4809
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.0708
_refine_diff_density_max         3.025
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0616P)^2^+18.4310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3951
_reflns_number_total             4520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03972a2.cif
_cod_data_source_block           oajvlc
_cod_depositor_comments
'Adding full bibliography for 7705994--7706001.cif.'
_cod_database_code               7705998
_nottingham_internal_coll_name   OAJVLC
_nottingham_internal_coll_number 15517
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '4.0000, 1.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   25/01/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_process_date 27/01/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 29/10/18
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 29/10/18
_nottingham_internal_refinement_user pcxav1
_nottingham_internal_self_archive_date 29/10/18
_nottingham_internal_self_validation_date 29/10/18
_nottingham_internal_self_validation_user pcxav1
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C25 H29 I Si'
_chemical_oxdiff_usercomment
'OAJVLC#15517 SN-840 in fomblin film on a micromount for AJV/DLK'
_shelx_estimated_absorpt_t_max   0.499
_shelx_estimated_absorpt_t_min   0.073
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              3512
_olex2_date_sample_data_collection 2016-01-27
_olex2_date_sample_submission    2016-01-25
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id OAJVLC
_olex2_submission_special_instructions 'No special instructions were received'