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_7705997
_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         'C50 H58 Li2 Si2'
_chemical_formula_sum            'C50 H58 Li2 Si2'
_chemical_formula_weight         729.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                69.756(4)
_cell_angle_beta                 85.404(4)
_cell_angle_gamma                64.756(4)
_cell_formula_units_Z            2
_cell_length_a                   11.7845(5)
_cell_length_b                   13.7778(6)
_cell_length_c                   16.2675(8)
_cell_measurement_reflns_used    7572
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.6570
_cell_measurement_theta_min      3.7600
_cell_volume                     2234.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      'N2 gas'
_diffrn_ambient_temperature      120(2)
_diffrn_crystal_treatment        'flash frozen in gaseous N2'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 4.2207
_diffrn_detector_type            'Agilent Diffraction Titan S2 detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_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     21.00  47.00   1.00   22.50    --   43.31  38.00 -90.00   26
  2  \w     70.00  96.00   1.00   22.50    --   43.31  38.00 -90.00   26
  3  \w    102.00 156.00   1.00   90.00    --  103.00  77.00-180.00   54
  4  \w     99.00 153.00   1.00   90.00    --  103.00  30.00-180.00   54
  5  \w     63.00 109.00   1.00   90.00    --  103.00 -94.00-120.00   46
  6  \w     65.00 121.00   1.00   90.00    --  103.00-125.00-180.00   56
  7  \w     64.00  90.00   1.00   90.00    --  103.00 -45.00-150.00   26
  8  \w     42.00 108.00   1.00   90.00    --  103.00 -94.00 -30.00   66
  9  \w     53.00  90.00   1.00   90.00    --  103.00 -30.00  60.00   37
 10  \w     80.00 176.00   1.00   90.00    --  103.00  30.00  90.00   96
 11  \w     51.00  96.00   1.00   90.00    --  103.00 -94.00  60.00   45
 12  \w     36.00  96.00   1.00   90.00    --  103.00 -45.00  30.00   60
 13  \w     30.00  78.00   1.00   90.00    --  103.00 -30.00 -90.00   48
 14  \w     30.00  84.00   1.00   90.00    --  103.00 -30.00-180.00   54
 15  \w      3.00  91.00   1.00   22.50    --   43.31-125.00 -30.00   88
 16  \w     23.00  72.00   1.00   90.00    --  103.00 -94.00  30.00   49
 17  \w     35.00  99.00   1.00   90.00    --  103.00 -61.00 150.00   64
 18  \w   -109.00 -21.00   1.00   22.50    --  -43.31 -57.00  30.00   88
 19  \w   -115.00 -13.00   1.00   22.50    --  -43.31 -77.00 150.00  102
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Titan S2'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0293349000
_diffrn_orient_matrix_UB_12      0.1264163000
_diffrn_orient_matrix_UB_13      -0.0197673000
_diffrn_orient_matrix_UB_21      0.0461496000
_diffrn_orient_matrix_UB_22      0.0087776000
_diffrn_orient_matrix_UB_23      -0.0924946000
_diffrn_orient_matrix_UB_31      -0.1342820000
_diffrn_orient_matrix_UB_32      0.0360561000
_diffrn_orient_matrix_UB_33      -0.0361575000
_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  0.0335
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16819
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.801
_diffrn_reflns_theta_min         2.904
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.084
_exptl_crystal_description       block
_exptl_crystal_F_000             784
_exptl_crystal_recrystallization_method 'Recrystallised from hexane at -30'
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         8737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0456P)^2^+1.1995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1148
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7313
_reflns_number_total             8737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03972a2.cif
_cod_data_source_block           liajvg
_cod_depositor_comments
'Adding full bibliography for 7705994--7706001.cif.'
_cod_original_cell_volume        2234.36(19)
_cod_database_code               7705997
_nottingham_internal_coll_name   LIAJVG
_nottingham_internal_coll_number 16622
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '90.00, 22.50'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   02/11/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVA, PL13110002'
_nottingham_internal_process_date 09/11/2018
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 09/11/2018
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 09/11/2018
_nottingham_internal_refinement_user pcxav1
_nottingham_internal_self_archive_date 09/11/2018
_nottingham_internal_self_validation_date 09/11/2018
_nottingham_internal_self_validation_user pcxav1
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H58 Li2 Si2'
_chemical_oxdiff_usercomment
'LIAJVG #16622 GVA-1104 IN FOMBLIN FILM ON MICROMOUNT FOR AJV/DLK'
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.832
_reflns_odcompleteness_completeness 99.81
_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),
 C25(H25), C27(H27), C31(H31), C32(H32), C33(H33), C39(H39), C40(H40), C41(H41)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              22420
_olex2_date_sample_data_collection 2016-11-02
_olex2_date_sample_submission    2016-10-28
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_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 1.504
_oxdiff_exptl_absorpt_empirical_full_min 0.708