#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/39/7003975.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7003975
loop_
_publ_author_name
'Dureen, Meghan A.'
'Stephan, Douglas W.'
_publ_section_title
;
 Biphenylamide ligand complexes of Li and Al: hemilabile arene donors?
;
_journal_issue                   35
_journal_name_full               'Dalton Transactions'
_journal_page_first              4723
_journal_page_last               4731
_journal_paper_doi               10.1039/b801772g
_journal_year                    2008
_chemical_formula_sum            'C24 H19 N'
_chemical_formula_weight         321.40
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.782(3)
_cell_length_b                   12.569(3)
_cell_length_c                   23.822(6)
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3527.8(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27103
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.613290
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.028
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0444P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0980
_reflns_number_gt                1773
_reflns_number_total             2524
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801772g.txt
_cod_data_source_block           (C6H4Ph)2NH
_cod_original_cell_volume        3527.8(16)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7003975
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.17107(15) 0.91114(13) 0.13244(7) 0.0628(5) Uani 1 1 d . . .
H1A H 0.1557 0.9602 0.1565 0.075 Uiso 1 1 calc R . .
C2 C 0.17954(15) 1.03482(14) 0.05330(7) 0.0449(5) Uani 1 1 d . . .
C3 C 0.30285(18) 0.88219(16) 0.05560(9) 0.0598(6) Uani 1 1 d . . .
H3A H 0.3272 0.8202 0.0732 0.072 Uiso 1 1 calc R . .
C4 C 0.16266(16) 0.77160(15) 0.20316(8) 0.0497(5) Uani 1 1 d . . .
C5 C 0.14901(16) 0.80572(15) 0.14750(8) 0.0503(5) Uani 1 1 d . . .
C6 C 0.21717(16) 0.94218(15) 0.08001(8) 0.0492(5) Uani 1 1 d . . .
C7 C 0.08764(16) 1.10352(13) 0.07640(8) 0.0462(5) Uani 1 1 d . . .
C8 C 0.10928(17) 0.73382(17) 0.10758(9) 0.0602(6) Uani 1 1 d . . .
H8A H 0.0987 0.7565 0.0708 0.072 Uiso 1 1 calc R . .
C9 C 0.09103(17) 1.14481(14) 0.13031(8) 0.0504(5) Uani 1 1 d . . .
H9A H 0.1505 1.1262 0.1540 0.060 Uiso 1 1 calc R . .
C10 C 0.23145(17) 1.06333(16) 0.00306(8) 0.0559(5) Uani 1 1 d . . .
H10A H 0.2075 1.1248 -0.0152 0.067 Uiso 1 1 calc R . .
C11 C 0.00790(18) 1.21309(16) 0.14947(9) 0.0605(6) Uani 1 1 d . . .
H11A H 0.0119 1.2404 0.1857 0.073 Uiso 1 1 calc R . .
C12 C -0.00278(18) 1.13327(15) 0.04229(8) 0.0570(6) Uani 1 1 d . . .
H12A H -0.0069 1.1074 0.0058 0.068 Uiso 1 1 calc R . .
C13 C 0.31685(19) 1.00387(19) -0.02058(9) 0.0653(6) Uani 1 1 d . . .
H13A H 0.3502 1.0251 -0.0541 0.078 Uiso 1 1 calc R . .
C14 C 0.20804(17) 0.84243(16) 0.24773(8) 0.0511(5) Uani 1 1 d . . .
C15 C 0.10016(19) 0.59556(17) 0.17578(11) 0.0697(6) Uani 1 1 d . . .
H15A H 0.0851 0.5252 0.1853 0.084 Uiso 1 1 calc R . .
C16 C 0.35242(19) 0.91254(17) 0.00597(9) 0.0651(6) Uani 1 1 d . . .
H16A H 0.4099 0.8715 -0.0097 0.078 Uiso 1 1 calc R . .
C17 C 0.13741(18) 0.66617(16) 0.21585(9) 0.0606(6) Uani 1 1 d . . .
H17A H 0.1460 0.6427 0.2526 0.073 Uiso 1 1 calc R . .
C18 C -0.08652(19) 1.20056(17) 0.06176(10) 0.0670(6) Uani 1 1 d . . .
H18A H -0.1470 1.2186 0.0385 0.080 Uiso 1 1 calc R . .
C19 C 0.15248(19) 0.93419(16) 0.26478(8) 0.0595(6) Uani 1 1 d . . .
H19A H 0.0856 0.9542 0.2469 0.071 Uiso 1 1 calc R . .
C20 C -0.08108(19) 1.24080(17) 0.11482(10) 0.0665(6) Uani 1 1 d . . .
H20A H -0.1372 1.2868 0.1276 0.080 Uiso 1 1 calc R . .
C21 C 0.30733(19) 0.81595(19) 0.27572(9) 0.0698(7) Uani 1 1 d . . .
H21A H 0.3462 0.7546 0.2655 0.084 Uiso 1 1 calc R . .
C22 C 0.08538(18) 0.62978(18) 0.12149(10) 0.0660(6) Uani 1 1 d . . .
H22A H 0.0593 0.5829 0.0942 0.079 Uiso 1 1 calc R . .
C23 C 0.1946(2) 0.99651(19) 0.30784(9) 0.0725(7) Uani 1 1 d . . .
H23A H 0.1554 1.0572 0.3190 0.087 Uiso 1 1 calc R . .
C24 C 0.3495(2) 0.8783(2) 0.31827(10) 0.0828(7) Uani 1 1 d . . .
H24A H 0.4163 0.8587 0.3364 0.099 Uiso 1 1 calc R . .
C25 C 0.2942(2) 0.9690(2) 0.33424(10) 0.0806(7) Uani 1 1 d . . .
H25A H 0.3237 1.0117 0.3626 0.097 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 N1 C6 123.97(16) . . ?
C10 C2 C6 117.80(18) . . ?
C10 C2 C7 119.21(16) . . ?
C6 C2 C7 122.99(17) . . ?
C16 C3 C6 121.29(19) . . ?
C17 C4 C5 118.17(19) . . ?
C17 C4 C14 119.50(18) . . ?
C5 C4 C14 122.26(18) . . ?
C8 C5 N1 120.18(18) . . ?
C8 C5 C4 119.04(18) . . ?
N1 C5 C4 120.75(18) . . ?
C3 C6 C2 119.49(18) . . ?
C3 C6 N1 119.91(17) . . ?
C2 C6 N1 120.57(17) . . ?
C9 C7 C12 117.56(18) . . ?
C9 C7 C2 122.57(17) . . ?
C12 C7 C2 119.77(17) . . ?
C22 C8 C5 121.3(2) . . ?
C11 C9 C7 121.27(19) . . ?
C13 C10 C2 122.31(19) . . ?
C20 C11 C9 119.9(2) . . ?
C18 C12 C7 121.07(19) . . ?
C10 C13 C16 119.2(2) . . ?
C21 C14 C19 117.2(2) . . ?
C21 C14 C4 120.23(19) . . ?
C19 C14 C4 122.54(19) . . ?
C22 C15 C17 119.5(2) . . ?
C3 C16 C13 119.9(2) . . ?
C15 C17 C4 122.1(2) . . ?
C20 C18 C12 120.4(2) . . ?
C23 C19 C14 121.3(2) . . ?
C18 C20 C11 119.8(2) . . ?
C24 C21 C14 121.5(2) . . ?
C15 C22 C8 119.8(2) . . ?
C25 C23 C19 120.2(2) . . ?
C25 C24 C21 120.6(2) . . ?
C24 C25 C23 119.3(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C5 1.397(2) . ?
N1 C6 1.417(2) . ?
C2 C10 1.391(3) . ?
C2 C6 1.399(2) . ?
C2 C7 1.490(2) . ?
C3 C16 1.373(3) . ?
C3 C6 1.388(3) . ?
C4 C17 1.392(3) . ?
C4 C5 1.403(3) . ?
C4 C14 1.485(3) . ?
C5 C8 1.393(3) . ?
C7 C9 1.386(2) . ?
C7 C12 1.391(3) . ?
C8 C22 1.378(3) . ?
C9 C11 1.380(3) . ?
C10 C13 1.374(3) . ?
C11 C20 1.379(3) . ?
C12 C18 1.380(3) . ?
C13 C16 1.376(3) . ?
C14 C21 1.387(3) . ?
C14 C19 1.387(3) . ?
C15 C22 1.374(3) . ?
C15 C17 1.375(3) . ?
C18 C20 1.363(3) . ?
C19 C23 1.383(3) . ?
C21 C24 1.375(3) . ?
C23 C25 1.376(3) . ?
C24 C25 1.367(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 28416213
