#------------------------------------------------------------------------------
#$Date: 2019-11-28 15:39:27 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244051 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/28/7702853.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_7702853
loop_
_publ_author_name
'Baker, Robert J.'
'Farley, Robert D.'
'Jones, Cameron'
'Kloth, Marc'
'Murphy, Damien M.'
_publ_section_title
;
 The reactivity of diazabutadienes toward low oxidation state Group 13
 iodides and the synthesis of a new gallium(i) carbene analogue
;
_journal_issue                   20
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3844
_journal_paper_doi               10.1039/b206605j
_journal_year                    2002
_chemical_formula_sum            'C26 H36 Al I2 N2'
_chemical_formula_weight         657.35
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m 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            4
_cell_length_a                   12.564(3)
_cell_length_b                   21.284(4)
_cell_length_c                   10.412(2)
_cell_measurement_temperature    150(2)
_cell_volume                     2784.3(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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    0.0286
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            47890
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    2.306
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.60
_exptl_absorpt_correction_type   'Sortav (Blessing)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0299P)²+1.7133P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0643
_reflns_number_gt                2797
_reflns_number_total             3273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206605j.txt
_cod_data_source_block           compound9
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7702853
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -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
I1 I -0.366467(18) 0.2500 0.07385(2) 0.02743(8) Uani 1 2 d S
I2 I -0.198339(18) 0.2500 0.41558(2) 0.02770(8) Uani 1 2 d S
Al1 Al -0.18558(8) 0.2500 0.17290(10) 0.0191(2) Uani 1 2 d S
N1 N -0.08916(15) 0.31133(9) 0.11240(18) 0.0181(4) Uani 1 1 d .
C1 C 0.0017(2) 0.28309(12) 0.0787(2) 0.0202(5) Uani 1 1 d .
H1 H 0.0620 0.3060 0.0564 0.024 Uiso 1 1 calc R
C2 C -0.10389(19) 0.37770(11) 0.0892(2) 0.0190(5) Uani 1 1 d .
C3 C -0.14616(19) 0.39613(11) -0.0305(2) 0.0209(5) Uani 1 1 d .
C4 C -0.1650(2) 0.45978(13) -0.0499(2) 0.0266(6) Uani 1 1 d .
H4 H -0.1934 0.4732 -0.1278 0.032 Uiso 1 1 calc R
C5 C -0.1424(2) 0.50369(12) 0.0445(3) 0.0291(6) Uani 1 1 d .
H5 H -0.1566 0.5460 0.0302 0.035 Uiso 1 1 calc R
C6 C -0.0989(2) 0.48468(12) 0.1591(3) 0.0272(6) Uani 1 1 d .
H6 H -0.0827 0.5147 0.2209 0.033 Uiso 1 1 calc R
C7 C -0.07846(19) 0.42156(11) 0.1853(2) 0.0207(5) Uani 1 1 d .
C8 C -0.1636(2) 0.34886(13) -0.1384(2) 0.0268(6) Uani 1 1 d .
H8 H -0.1720 0.3073 -0.0993 0.032 Uiso 1 1 calc R
C9 C -0.2634(3) 0.36241(16) -0.2171(3) 0.0426(7) Uani 1 1 d .
H9A H -0.3235 0.3660 -0.1608 0.064 Uiso 1 1 calc R
H9B H -0.2751 0.3287 -0.2768 0.064 Uiso 1 1 calc R
H9C H -0.2542 0.4011 -0.2634 0.064 Uiso 1 1 calc R
C10 C -0.0650(3) 0.34670(15) -0.2255(3) 0.0391(7) Uani 1 1 d .
H10A H -0.0539 0.3873 -0.2634 0.059 Uiso 1 1 calc R
H10B H -0.0758 0.3162 -0.2921 0.059 Uiso 1 1 calc R
H10C H -0.0038 0.3353 -0.1755 0.059 Uiso 1 1 calc R
C11 C -0.0266(2) 0.40265(13) 0.3109(2) 0.0267(6) Uani 1 1 d .
H11 H -0.0257 0.3566 0.3150 0.032 Uiso 1 1 calc R
C12 C -0.0892(3) 0.42685(15) 0.4271(2) 0.0437(8) Uani 1 1 d .
H12A H -0.0877 0.4719 0.4279 0.066 Uiso 1 1 calc R
H12B H -0.0574 0.4111 0.5046 0.066 Uiso 1 1 calc R
H12C H -0.1615 0.4126 0.4216 0.066 Uiso 1 1 calc R
C13 C 0.0886(2) 0.42565(15) 0.3155(3) 0.0413(8) Uani 1 1 d .
H13A H 0.1274 0.4083 0.2444 0.062 Uiso 1 1 calc R
H13B H 0.1209 0.4124 0.3946 0.062 Uiso 1 1 calc R
H13C H 0.0898 0.4707 0.3104 0.062 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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
N1 Al1 N1 87.42(13) . 8_565
N1 Al1 I1 116.50(7) . .
N1 Al1 I1 116.50(7) 8_565 .
N1 Al1 I2 111.93(7) . .
N1 Al1 I2 111.93(7) 8_565 .
I1 Al1 I2 110.78(4) . .
C1 N1 C2 120.3(2) . .
C1 N1 Al1 108.93(17) . .
C2 N1 Al1 130.47(16) . .
N1 C1 C1 116.71(14) . 8_565
C7 C2 C3 122.0(2) . .
C7 C2 N1 120.1(2) . .
C3 C2 N1 117.9(2) . .
C4 C3 C2 117.6(2) . .
C4 C3 C8 120.8(2) . .
C2 C3 C8 121.5(2) . .
C5 C4 C3 121.2(2) . .
C6 C5 C4 120.0(2) . .
C5 C6 C7 121.8(2) . .
C6 C7 C2 117.3(2) . .
C6 C7 C11 120.2(2) . .
C2 C7 C11 122.4(2) . .
C3 C8 C9 112.9(2) . .
C3 C8 C10 109.8(2) . .
C9 C8 C10 110.6(2) . .
C7 C11 C13 110.4(2) . .
C7 C11 C12 111.8(2) . .
C13 C11 C12 110.7(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Al1 2.4957(11) .
I2 Al1 2.5318(11) .
Al1 N1 1.889(2) .
Al1 N1 1.889(2) 8_565
N1 C1 1.337(3) .
N1 C2 1.445(3) .
C1 C1 1.409(5) 8_565
C2 C7 1.405(3) .
C2 C3 1.411(3) .
C3 C4 1.390(4) .
C3 C8 1.524(3) .
C4 C5 1.386(4) .
C5 C6 1.373(4) .
C6 C7 1.395(3) .
C7 C11 1.516(3) .
C8 C9 1.525(4) .
C8 C10 1.536(4) .
C11 C13 1.529(4) .
C11 C12 1.532(4) .
