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_7706000
_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         'C52 H58 Li2'
_chemical_formula_sum            'C52 H58 Li2'
_chemical_formula_weight         696.86
_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             2020-07-02
_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                113.742(6)
_cell_angle_beta                 101.077(4)
_cell_angle_gamma                104.484(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9982(4)
_cell_length_b                   15.2538(10)
_cell_length_c                   15.4697(9)
_cell_measurement_reflns_used    8513
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4270
_cell_measurement_theta_min      4.1310
_cell_volume                     2368.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.970
_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     61.00 178.00   1.00    6.00    --  106.13  15.00 120.00  117
  2  \w     79.00 119.00   1.00    6.00    --  106.13-125.00 -30.00   40
  3  \w     62.00  97.00   1.00    6.00    --  106.13 -45.00 -60.00   35
  4  \w     50.00  83.00   1.00    6.00    --  106.13 -30.00 -90.00   33
  5  \w     94.00 177.00   1.00    6.00    --  106.13  30.00-180.00   83
  6  \w     66.00  96.00   1.00    1.50    --   43.22-125.00-180.00   30
  7  \w     52.00  83.00   1.00    6.00    --  106.13 -30.00-180.00   31
  8  \w     28.00  97.00   1.00    6.00    --  106.13 -95.00 -30.00   69
  9  \w     62.00  89.00   1.00    6.00    --  106.13 -30.00  30.00   27
 10  \w     35.00 100.00   1.00    6.00    --  106.13 -95.00  90.00   65
 11  \w     74.00 104.00   1.00    6.00    --  106.13 -95.00 150.00   30
 12  \w     54.00 119.00   1.00    6.00    --  106.13-125.00  90.00   65
 13  \w     44.00 129.00   1.00    6.00    --  106.13 -77.00 150.00   85
 14  \w     31.00  82.00   1.00    6.00    --  106.13 -30.00 150.00   51
 15  \w     30.00  60.00   1.00    6.00    --  106.13 -95.00 150.00   30
 16  \w     23.00  88.00   1.00    1.50    --   43.22-125.00  90.00   65
 17  \w     35.00  73.00   1.00    6.00    --  106.13-125.00 -30.00   38
 18  \w    -71.00  39.00   1.00    1.50    --  -38.50  19.00 -90.00  110
 19  \w    -47.00  34.00   1.00    1.50    --  -38.50  38.00 -30.00   81
 20  \w    -97.00 -16.00   1.00    1.50    --  -38.50 -38.00  90.00   81
;
_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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0067976000
_diffrn_orient_matrix_UB_12      0.0744820000
_diffrn_orient_matrix_UB_13      -0.0444159000
_diffrn_orient_matrix_UB_21      0.0064710000
_diffrn_orient_matrix_UB_22      -0.0812732000
_diffrn_orient_matrix_UB_23      -0.0964810000
_diffrn_orient_matrix_UB_31      -0.1401907000
_diffrn_orient_matrix_UB_32      -0.0434283000
_diffrn_orient_matrix_UB_33      -0.0447762000
_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  0.0213
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18068
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.363
_diffrn_reflns_theta_min         3.307
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.399
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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    0.977
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.615
_exptl_crystal_size_mid          0.346
_exptl_crystal_size_min          0.219
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         9359
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0752P)^2^+0.4271P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8068
_reflns_number_total             9359
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03972a2.cif
_cod_data_source_block           liajvb_sq
_cod_depositor_comments
'Adding full bibliography for 7705994--7706001.cif.'
_cod_original_cell_volume        2368.3(2)
_cod_database_code               7706000
_nottingham_internal_coll_name   LIAJVB
_nottingham_internal_coll_number 15492
_nottingham_internal_coll_client AJV/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 6.00, 1.50'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   21/01/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017/09'
_nottingham_internal_process_date 14/03/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 14/03/2016
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 29/04/2020
_nottingham_internal_refinement_user pcxav1/pczlt/pczspa
_nottingham_internal_validation_date 29/04/2020
_nottingham_internal_validation_user pczspa
_platon_squeeze_void_probe_radius 1.20
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C52 H58 Li2'
_chemical_oxdiff_usercomment
'LIAJVB #15492 SN-831 IN FOMBLIN FILM ON MICROMOUNT FOR AJV/DLK'
_shelx_estimated_absorpt_t_max   0.918
_shelx_estimated_absorpt_t_min   0.791
_reflns_odcompleteness_completeness 99.88
_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. Restrained distances
 C49A-C26 \\sim C49B-C26
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C49A \\sim C50A \\sim C51A \\sim C52A \\sim C49B \\sim C50B \\sim C51B \\sim
C52B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
Uanis(C49A) = Uanis(C49B)
Uanis(C52A) = Uanis(C52B)
4. Rigid body (RIGU) restrains
 C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49A, C50A, C51A, C52A, C49B, C50B, C51B, C52B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{C49A, C52A, C50A, C51A} sigma for 1-2: 0.02, 1-3: 0.04
{C49A, C52A, C51A, C50A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C49A, C50A, C51A, C52A}
{C49A, C50A, C51A, C52A} sigma for 1-2: 0.02, 1-3: 0.04
{C49A, C52A, C50A, C51A} sigma for 1-2: 0.02, 1-3: 0.04
{C49A, C52A, C51A, C50A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{C49B, C50B, C51B, C52B}
6. Others
 Sof(C49B)=Sof(C50B)=Sof(H50d)=Sof(H50e)=Sof(H50f)=Sof(C51B)=Sof(H51d)=
 Sof(H51e)=Sof(H51f)=Sof(C52B)=Sof(H52d)=Sof(H52e)=Sof(H52f)=1-FVAR(1)
 Sof(C49A)=Sof(C50A)=Sof(H50a)=Sof(H50b)=Sof(H50c)=Sof(C51A)=Sof(H51a)=
 Sof(H51b)=Sof(H51c)=Sof(C52A)=Sof(H52a)=Sof(H52b)=Sof(H52c)=FVAR(1)
7.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)
7.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), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C48(H48a,H48b,H48c),
 C50A(H50a,H50b,H50c), C51A(H51a,H51b,H51c), C52A(H52a,H52b,H52c), C50B(H50d,
 H50e,H50f), C51B(H51d,H51e,H51f), C52B(H52d,H52e,H52f)
;
_shelx_res_checksum              13932
_shelx_fab_checksum              74592
_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 1.446
_oxdiff_exptl_absorpt_empirical_full_min 0.563