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_7705994
_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         'C26 H29 I'
_chemical_formula_sum            'C26 H29 I'
_chemical_formula_weight         468.39
_chemical_name_systematic        OAJVLB
_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             2020-07-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-11-18 deposited with the CCDC.	2020-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.910(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1749(2)
_cell_length_b                   13.2712(2)
_cell_length_c                   13.8896(2)
_cell_measurement_reflns_used    5542
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.3950
_cell_measurement_theta_min      4.7400
_cell_volume                     2283.39(7)
_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 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 0.9993
_diffrn_measured_fraction_theta_max 0.9682
_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     90.00 178.00   1.00   10.00    --  104.50  30.00 120.00   88
  2  \w     59.00 162.00   1.00   10.00    --  104.50  15.00-120.00  103
  3  \w     46.00  91.00   1.00   10.00    --  104.50 -45.00-120.00   45
  4  \w     36.00 106.00   1.00   10.00    --  104.50 -94.00-180.00   70
  5  \w     28.00 106.00   1.00   10.00    --  104.50 -94.00  90.00   78
  6  \w     47.00  85.00   1.00   10.00    --  104.50 -45.00 150.00   38
  7  \w    -43.00   8.00   1.00    2.50    --  -38.50  38.00 -60.00   51
  8  \w    -46.00 -12.00   1.00    2.50    --  -38.50  38.00 -90.00   34
  9  \w    -68.00 -42.00   1.00    2.50    --  -38.50  77.00 -90.00   26
 10  \w   -108.00 -12.00   1.00    2.50    --  -38.50 -57.00 -60.00   96
;
_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      0.0815210000
_diffrn_orient_matrix_UB_12      0.0047337000
_diffrn_orient_matrix_UB_13      0.1099416000
_diffrn_orient_matrix_UB_21      -0.0939117000
_diffrn_orient_matrix_UB_22      0.0025900000
_diffrn_orient_matrix_UB_23      0.0423352000
_diffrn_orient_matrix_UB_31      0.0011913000
_diffrn_orient_matrix_UB_32      -0.1159825000
_diffrn_orient_matrix_UB_33      0.0054394000
_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  0.0240
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.580
_diffrn_reflns_theta_min         3.996
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.046
_exptl_absorpt_correction_T_max  0.636
_exptl_absorpt_correction_T_min  0.411
_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    1.362
_exptl_crystal_description       block
_exptl_crystal_F_000             1060.000
_exptl_crystal_recrystallization_method 'Recrystallised from ethanol.'
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.386
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4470
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0333P)^2^+1.0914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4017
_reflns_number_total             4470
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03972a2.cif
_cod_data_source_block           oajvlb
_cod_depositor_comments
'Adding full bibliography for 7705994--7706001.cif.'
_cod_original_cell_volume        2283.39(6)
_cod_database_code               7705994
_nottingham_internal_coll_name   OAJVLB
_nottingham_internal_coll_number 15456
_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,, 10.00, 2.50'
_nottingham_internal_coll_frame_width 'in, 1.00'
_nottingham_internal_coll_user   pcxav1
_nottingham_internal_coll_date   18/01/2016
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVB, PL13110001'
_nottingham_internal_process_date 29/02/2016
_nottingham_internal_process_user pcxav1
_nottingham_internal_solution_date 26/10/16
_nottingham_internal_solution_user pcxav1
_nottingham_internal_refinement_date 26/10/16
_nottingham_internal_refinement_user pcxav1/pczspa
_nottingham_internal_self_archive_date 26/10/16
_nottingham_internal_self_validation_date 26/10/16
_nottingham_internal_self_validation_user pcxav1
_nottingham_internal_validation_date 28/04/2020
_nottingham_internal_validation_user pczspa
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C26 H29 I1'
_chemical_oxdiff_usercomment
'OAJVLB #15456 GVB-854 IN FOMBLIN FILM ON MICROMOUNT FOR AJV/DLK'
_shelx_estimated_absorpt_t_max   0.597
_shelx_estimated_absorpt_t_min   0.311
_reflns_odcompleteness_completeness 99.93
_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
 C25-C23 \\sim C26-C23 \\sim C24-C23
 with sigma of 0.02
 C24-C25 \\sim C25-C26 \\sim C26-C24
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C24, C23
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C17(H17), C18(H18), C19(H19)
5.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              631
_olex2_date_sample_data_collection 2015-01-14
_olex2_date_sample_submission    2015-01-07
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_original_sample_id OAJVLB
_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 1.574
_oxdiff_exptl_absorpt_empirical_full_min 0.687