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_7705999
_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         'C44 H40 Cl2 Li2, 0.5(C6 H14)'
_chemical_formula_sum            'C47 H47 Cl2 Li2'
_chemical_formula_weight         696.62
_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                 103.471(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1125(11)
_cell_length_b                   16.8343(14)
_cell_length_c                   19.6420(14)
_cell_measurement_reflns_used    3993
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.2590
_cell_measurement_theta_min      3.4720
_cell_volume                     3894.9(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 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 area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.958
_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    -50.00  34.00   1.00   60.00    --  -38.50  38.00  30.00   84
  2  \w    -50.00  34.00   1.00   60.00    --  -38.50  38.00 150.00   84
  3  \w    -50.00  34.00   1.00   60.00    --  -38.50  38.00 -90.00   84
  4  \w      1.00  83.00   1.00   60.00    --   43.32 -99.00  60.00   82
  5  \w     23.00  98.00   1.00   60.00    --   43.32-125.00 -90.00   75
  6  \w     35.00  98.00   1.00  240.00    --  106.13 -45.00  90.00   63
  7  \w     25.00 109.00   1.00  240.00    --  106.13 -95.00  30.00   84
  8  \w     57.00  91.00   1.00  240.00    --  106.13 -30.00   0.00   34
  9  \w     93.00 172.00   1.00  240.00    --  106.13  30.00-150.00   79
 10  \w     99.00 172.00   1.00  240.00    --  106.13 125.00-120.00   73
 11  \w     95.00 156.00   1.00  240.00    --  106.13 125.00  30.00   61
 12  \w     32.00  57.00   1.00  240.00    --  106.13 -30.00 -90.00   25
 13  \w     46.00  92.00   1.00  240.00    --  106.13 -45.00 150.00   46
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, 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      -0.1246974000
_diffrn_orient_matrix_UB_12      0.0139070000
_diffrn_orient_matrix_UB_13      -0.0383290000
_diffrn_orient_matrix_UB_21      -0.0333321000
_diffrn_orient_matrix_UB_22      -0.0792592000
_diffrn_orient_matrix_UB_23      0.0289791000
_diffrn_orient_matrix_UB_31      -0.0208515000
_diffrn_orient_matrix_UB_32      0.0436083000
_diffrn_orient_matrix_UB_33      0.0647998000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_unetI/netI     0.0718
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20656
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.806
_diffrn_reflns_theta_min         3.500
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.720
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.188
_exptl_crystal_description       block
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.051
_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     498
_refine_ls_number_reflns         7768
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0705
_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^)+(0.0662P)^2^+2.6019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4536
_reflns_number_total             7768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03972a2.cif
_cod_data_source_block           kewjmb
_cod_depositor_comments
'Adding full bibliography for 7705994--7706001.cif.'
_cod_database_code               7705999
_nottingham_internal_coll_name   KEWJMB
_nottingham_internal_coll_number 16697
_nottingham_internal_coll_client KEW/JM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_frame_time '240.00, 60.00'
_nottingham_internal_coll_frame_width 1.00
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   22/11/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'SN, XDA 017-09'
_nottingham_internal_process_date 25/11/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 06/12/16
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 06/12/16
_nottingham_internal_refinement_user pczwl/pcxav1
_nottingham_internal_self_archive_date 06/12/16
_nottingham_internal_self_validation_date 06/12/16
_nottingham_internal_self_validation_user pcxav1
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H20 Cl Li'
_chemical_oxdiff_usercomment
'KEWJMB#16697 SN-1096 IN FOMBLIN FILM ON MICROMOUNT FOR KEW/JM'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46-C45 \\sim C50-C48 \\sim C48-C49 \\sim C46-C47 \\sim C48-C47
 with sigma of 0.02
 C45-C47 \\sim C46-C48 \\sim C47-C49 \\sim C47-C50 \\sim C49-C50
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 C45, C46, C47, C48, C49, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C45(0.5) H45a(0.5) H45b(0.5) H45c(0.5) C46(0.5) H46a(0.5)
 H46b(0.5) C47(0.5) H47a(0.5) H47b(0.5) C48(0.5) H48(0.5) C49(0.5) H49a(0.5)
 H49b(0.5) H49c(0.5) C50(0.5) H50a(0.5) H50b(0.5) H50c(0.5)
6.a Ternary CH refined with riding coordinates:
 C48(H48)
6.b Secondary CH2 refined with riding coordinates:
 C46(H46a,H46b), C47(H47a,H47b)
6.c 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)
6.d 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), C49(H49a,H49b,H49c), C50(H50a,H50b,H50c)
;
_shelx_res_checksum              5071
_olex2_date_sample_data_collection 2016-11-22
_olex2_date_sample_submission    2016-11-21
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id KEWJMB
_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 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.756