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_7705995
_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         'C22 H20 Cl I'
_chemical_formula_sum            'C22 H20 Cl I'
_chemical_formula_weight         446.73
_chemical_name_systematic        KEWJMA
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 100.064(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.3499(2)
_cell_length_b                   34.7269(7)
_cell_length_c                   13.4766(3)
_cell_measurement_reflns_used    9412
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.5030
_cell_measurement_theta_min      4.2040
_cell_volume                     3847.63(15)
_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 plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.9971
_diffrn_measured_fraction_theta_max 0.9712
_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     38.00  64.00   1.00    2.00    --   42.83 -57.00 -60.00   26
  2  \w     81.00 170.00   1.00    8.00    --  104.50  30.00-180.00   89
  3  \w    124.00 150.00   1.00    8.00    --  104.50  45.00 -90.00   26
  4  \w     74.00 157.00   1.00    8.00    --  104.50 125.00-180.00   83
  5  \w     74.00 138.00   1.00    8.00    --  104.50  77.00-120.00   64
  6  \w     57.00  91.00   1.00    8.00    --  104.50 -30.00 -60.00   34
  7  \w     36.00  88.00   1.00    8.00    --  104.50 -30.00  30.00   52
  8  \w     63.00  89.00   1.00    8.00    --  104.50 -30.00 120.00   26
  9  \w     30.00 109.00   1.00    8.00    --  104.50 -94.00-180.00   79
 10  \w    -85.00 -20.00   1.00    2.00    --  -38.50 125.00-180.00   65
 11  \w   -111.00 -85.00   1.00    2.00    --  -38.50 -19.00 150.00   26
 12  \w   -111.00  -8.00   1.00    2.00    --  -38.50 -77.00  90.00  103
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_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      0.0937021000
_diffrn_orient_matrix_UB_12      0.0346178000
_diffrn_orient_matrix_UB_13      0.0529531000
_diffrn_orient_matrix_UB_21      0.0479434000
_diffrn_orient_matrix_UB_22      0.0124199000
_diffrn_orient_matrix_UB_23      -0.1006144000
_diffrn_orient_matrix_UB_31      -0.1550079000
_diffrn_orient_matrix_UB_32      0.0247939000
_diffrn_orient_matrix_UB_33      -0.0236351000
_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  0.0427
_diffrn_reflns_av_unetI/netI     0.0501
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16211
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.699
_diffrn_reflns_theta_min         3.566
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.332
_exptl_absorpt_correction_T_max  0.458
_exptl_absorpt_correction_T_min  0.068
_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    1.542
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_recrystallization_method
'Crystallised from diethyl ether via slow evaporation of the solvent.'
_exptl_crystal_size_max          0.649
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.171
_refine_diff_density_min         -1.323
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         7564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0640P)^2^+1.9549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6945
_reflns_number_total             7564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03972a2.cif
_cod_data_source_block           kewjma
_cod_depositor_comments
'Adding full bibliography for 7705994--7706001.cif.'
_cod_database_code               7705995
_nottingham_internal_coll_name   KEWJMA
_nottingham_internal_coll_number 16648
_nottingham_internal_coll_client KEW/JM
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'ofand \w scans'
_nottingham_internal_coll_frame_time 'degrees,, 8.00, 2.00'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   09/11/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 09/11/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 09/11/2016
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 09/11/2016
_nottingham_internal_refinement_user pcxav1
_nottingham_internal_self_archive_date 09/11/2016
_nottingham_internal_self_validation_date 09/11/2016
_nottingham_internal_self_validation_user pcxav1
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C22 H20 Cl I'
_chemical_oxdiff_usercomment
'KEWJMA #16648 GVB-1221 IN FOMBLIN FILM ON MICROMOUNT FOR KEW/JM'
_shelx_estimated_absorpt_t_max   0.397
_shelx_estimated_absorpt_t_min   0.039
_reflns_odcompleteness_completeness 99.71
_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)
;
_shelx_res_checksum              63118
_olex2_date_sample_data_collection 2016-11-09
_olex2_date_sample_submission    2016-11-07
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id KEWJMA
_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 2.083
_oxdiff_exptl_absorpt_empirical_full_min 0.552