Ligand influences on homoleptic Group 12 m-terphenyl complexes.
Blundell, Toby J.; Hastings, Fiona R.; Gridley, Benjamin M.; Moxey, Graeme J.; Lewis, William; Blake, Alexander J.; Kays, Deborah L.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14257–14264; doi:10.1039/c4dt00647j

data_7032740
_publ_section_title
;
 Ligand influences on homoleptic Group 12 m-terphenyl complexes.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14257
_journal_page_last               14264
_journal_paper_doi               10.1039/c4dt00647j
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C44 H42 Li2'
_chemical_formula_sum            'C44 H42 Li2'
_chemical_formula_weight         584.65
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.596(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.6871(3)
_cell_length_b                   42.4827(9)
_cell_length_c                   15.9595(4)
_cell_measurement_reflns_used    12547
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      69.2540
_cell_measurement_theta_min      4.2440
_cell_volume                     6944.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.0750
_diffrn_measured_fraction_theta_full 0.9947
_diffrn_measured_fraction_theta_max 0.9838
_diffrn_measurement_details
;
  1 omega  -80.00  -36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 44

  2 omega -116.00  -81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  178.0000   60.0000 35

  3 omega  -71.00  -45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000  -57.0000 -150.0000 26

  4 omega  -49.00   36.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -33.5000   38.0000 -120.0000 85

  5 omega    2.00   53.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000   60.0000 51

  6 omega   68.00  120.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   77.0000    0.0000 52

  7 omega    4.00   65.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000 -120.0000 61

  8 omega   32.00  122.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000  -30.0000 90

  9 omega   57.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -99.0000   60.0000 34

 10 omega   37.00   87.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 50

 11 omega   35.00   82.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -120.0000 47

 12 omega   32.00  112.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -12.0000 -150.0000 80

 13 omega   42.00  149.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -92.0000   90.0000 107

 14 omega  124.00  150.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   60.0000 26

 15 omega   36.00  103.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000  -60.0000 67

 16 omega   49.00   75.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -120.0000 26

 17 omega   47.00   73.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -150.0000 26

 18 omega   49.00   75.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  120.0000 26

 19 omega   88.00  113.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   12.0000  -90.0000 25

 20 omega  149.00  175.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   12.0000  -90.0000 26

 21 omega   49.00  116.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 67

 22 omega   83.00  109.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   30.0000 26

 23 omega   33.00   74.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -180.0000 41

 24 omega  133.00  177.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -12.0000  -90.0000 44

 25 omega   50.00  128.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -12.0000  -90.0000 78
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0763598000
_diffrn_orient_matrix_UB_12      -0.0287786000
_diffrn_orient_matrix_UB_13      -0.0469949000
_diffrn_orient_matrix_UB_21      -0.1130345000
_diffrn_orient_matrix_UB_22      0.0217060000
_diffrn_orient_matrix_UB_23      -0.0483998000
_diffrn_orient_matrix_UB_31      0.0632976000
_diffrn_orient_matrix_UB_32      0.0040491000
_diffrn_orient_matrix_UB_33      -0.0747904000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30836
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.071
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  1.212
_exptl_absorpt_correction_T_min  0.987
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.3398
_exptl_crystal_size_mid          0.2307
_exptl_crystal_size_min          0.1218
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     975
_refine_ls_number_reflns         12192
_refine_ls_number_restraints     1167
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0745
_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^)+(0.0380P)^2^+11.7159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1817
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10029
_reflns_number_total             12192
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00647j2.cif
_cod_data_source_block           4
_cod_database_code               7032740
_nottingham_internal_coll_name   LITBLA
_nottingham_internal_coll_number 12726
_nottingham_internal_coll_client TB/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time 10,20,80
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   TB
_nottingham_internal_coll_date   14/08/2013
_nottingham_internal_coll_location NOTT
_nottingham_internal_process_user TB
_nottingham_internal_process_date 07/03/2012
_nottingham_internal_solution_user TB
_nottingham_internal_solution_date 20/08/2013
_nottingham_internal_refinement_user TB
_nottingham_internal_refinement_date 20/08/2013
_nottingham_internal_validation_user wl
_nottingham_internal_validation_date 11/2/2014
_nottingham_internal_archive_date 11/2/2014
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C44 H42 Li2'
_chemical_oxdiff_usercomment
'LITBALA1 #12726 mounted in fomblin film on micromount for TB/DLK'
_reflns_odcompleteness_completeness 99.47
_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-C26 \\sim C26-C27 \\sim C25A-C26A \\sim C26A-C27A
 with sigma of 0.02
 C23-C24 \\sim C23-C28 \\sim C23A-C24A \\sim C23A-C28A
 with sigma of 0.02
 C24-C25 \\sim C27-C28 \\sim C24A-C25A \\sim C27A-C28A
 with sigma of 0.02
 C25-C26 \\sim C26-C27 \\sim C25A-C26A \\sim C26A-C27A
 with sigma of 0.02
 C24-C29 \\sim C24A-C29 \\sim C28-C37 \\sim C28A-C37
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C23A)=Sof(C24A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
 Sof(H27A)=Sof(C28A)=1-FVAR(1)
 Sof(C28)=Sof(C26)=Sof(H26)=Sof(C25)=Sof(H25)=Sof(C23)=Sof(C27)=Sof(H27)=
 Sof(C24)=FVAR(1)
 Sof(C81A)=Sof(C82A)=Sof(H82A)=Sof(C86A)=Sof(H86A)=Sof(C85A)=Sof(C84A)=
 Sof(H84A)=Sof(C83A)=Sof(C87A)=Sof(H87D)=Sof(H87E)=Sof(H87F)=Sof(C88A)=
 Sof(H88D)=Sof(H88E)=Sof(H88F)=1-FVAR(2)
 Sof(C81)=Sof(C82)=Sof(H82)=Sof(C83)=Sof(C84)=Sof(H84)=Sof(C85)=Sof(C86)=
 Sof(H86)=Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(H87C)=Sof(C88)=Sof(H88A)=Sof(H88B)=
 Sof(H88C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C12(H12), C16(H16), C18(H18),
 C20(H20), C30(H30), C32(H32), C34(H34), C38(H38), C40(H40), C42(H42), C47(H47),
  C48(H48), C49(H49), C52(H52), C54(H54), C56(H56), C60(H60), C62(H62),
 C64(H64), C69(H69), C70(H70), C71(H71), C74(H74), C76(H76), C78(H78), C82(H82),
  C84(H84), C86(H86), C26(H26), C25(H25), C27(H27), C25A(H25A), C26A(H26A),
 C27A(H27A), C82A(H82A), C86A(H86A), C84A(H84A)
5.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), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C79(H79A,H79B,H79C), C80(H80A,H80B,H80C), C87(H87A,H87B,
 H87C), C88(H88A,H88B,H88C), C87A(H87D,H87E,H87F), C88A(H88D,H88E,H88F)
;
_shelx_res_checksum              81562
_shelx_hkl_checksum              42992