#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:02:01 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180056 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/02/7050209.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_7050209
loop_
_publ_author_name
'Baker, Robert J.'
'Jones, Cameron'
'Kloth, Marc'
'Mills, David P.'
_publ_section_title
;
 The reactivity of gallium(i) and indium(i) halides towards
 bipyridines, terpyridines, imino-substituted pyridines and
 bis(imino)acenaphthenes
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              207
_journal_paper_doi               10.1039/b310592j
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C36 H44 Ga2 I4 N4'
_chemical_formula_weight         1179.79
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 124.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.813(5)
_cell_length_b                   14.364(3)
_cell_length_c                   17.672(4)
_cell_measurement_temperature    150(2)
_cell_volume                     4755(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21124
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    3.756
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing)'
_exptl_crystal_colour            yellow/green
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       0.00033(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         5406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0325
_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)+(0.0255P)²+8.3762P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0696
_refine_ls_wR_factor_ref         0.0736
_reflns_number_gt                4503
_reflns_number_total             5406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b310592j.txt
_cod_data_source_block           compound_5
_cod_original_cell_volume        4754.6(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050209
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
I1 I 0.215955(11) 0.476374(18) 0.460831(16) 0.03822(9) Uani 1 1 d . . .
I2 I 0.284822(13) 0.306409(19) 0.680328(17) 0.04165(10) Uani 1 1 d . . .
Ga1 Ga 0.325362(16) 0.42508(2) 0.61198(2) 0.02074(10) Uani 1 1 d . . .
N1 N 0.39626(13) 0.35446(18) 0.60479(17) 0.0201(5) Uani 1 1 d . . .
N2 N 0.39868(12) 0.51090(18) 0.68267(17) 0.0177(5) Uani 1 1 d . . .
C1 C 0.38648(18) 0.2708(2) 0.5646(2) 0.0302(8) Uani 1 1 d . . .
H1 H 0.3418 0.2428 0.5343 0.036 Uiso 1 1 calc R . .
C2 C 0.4405(2) 0.2259(3) 0.5673(2) 0.0351(8) Uani 1 1 d . . .
H2 H 0.4331 0.1682 0.5393 0.042 Uiso 1 1 calc R . .
C3 C 0.50685(19) 0.2692(2) 0.6132(2) 0.0318(8) Uani 1 1 d . . .
H3 H 0.5448 0.2399 0.6169 0.038 Uiso 1 1 calc R . .
C4 C 0.51662(16) 0.3553(2) 0.6532(2) 0.0236(7) Uani 1 1 d . . .
H4 H 0.5606 0.3851 0.6824 0.028 Uiso 1 1 calc R . .
C5 C 0.46014(15) 0.3969(2) 0.64932(19) 0.0172(6) Uani 1 1 d . . .
C6 C 0.46685(14) 0.4889(2) 0.69688(18) 0.0144(6) Uani 1 1 d . . .
H6 H 0.4760 0.5375 0.6659 0.017 Uiso 1 1 calc R . .
C7 C 0.38418(14) 0.6051(2) 0.6949(2) 0.0193(6) Uani 1 1 d . . .
C8 C 0.36429(15) 0.6226(2) 0.7559(2) 0.0238(7) Uani 1 1 d . . .
C9 C 0.35190(18) 0.7143(3) 0.7698(2) 0.0336(8) Uani 1 1 d . . .
H9 H 0.3392 0.7261 0.8104 0.040 Uiso 1 1 calc R . .
C10 C 0.35816(19) 0.7871(3) 0.7247(3) 0.0376(9) Uani 1 1 d . . .
H10 H 0.3519 0.8480 0.7366 0.045 Uiso 1 1 calc R . .
C11 C 0.37381(18) 0.7692(3) 0.6613(2) 0.0338(8) Uani 1 1 d . . .
H11 H 0.3772 0.8189 0.6303 0.041 Uiso 1 1 calc R . .
C12 C 0.38463(16) 0.6794(2) 0.6422(2) 0.0232(7) Uani 1 1 d . . .
C13 C 0.35287(19) 0.5459(3) 0.8052(2) 0.0336(8) Uani 1 1 d . . .
H13 H 0.3623 0.4867 0.7866 0.040 Uiso 1 1 calc R . .
C14 C 0.4044(3) 0.5523(4) 0.9103(3) 0.0607(13) Uani 1 1 d . . .
H14A H 0.4527 0.5507 0.9277 0.091 Uiso 1 1 calc R . .
H14B H 0.3964 0.5008 0.9379 0.091 Uiso 1 1 calc R . .
H14C H 0.3964 0.6096 0.9311 0.091 Uiso 1 1 calc R . .
C15 C 0.2748(2) 0.5434(3) 0.7749(4) 0.0623(14) Uani 1 1 d . . .
H15A H 0.2642 0.5994 0.7946 0.093 Uiso 1 1 calc R . .
H15B H 0.2679 0.4905 0.8022 0.093 Uiso 1 1 calc R . .
H15C H 0.2436 0.5386 0.7090 0.093 Uiso 1 1 calc R . .
C16 C 0.39100(16) 0.6663(2) 0.5620(2) 0.0261(7) Uani 1 1 d . . .
H16 H 0.3947 0.5995 0.5545 0.031 Uiso 1 1 calc R . .
C17 C 0.32449(19) 0.7033(3) 0.4718(2) 0.0371(9) Uani 1 1 d . . .
H17A H 0.2826 0.6745 0.4617 0.056 Uiso 1 1 calc R . .
H17B H 0.3279 0.6888 0.4214 0.056 Uiso 1 1 calc R . .
H17C H 0.3215 0.7695 0.4760 0.056 Uiso 1 1 calc R . .
C18 C 0.45771(19) 0.7133(3) 0.5797(3) 0.0407(9) Uani 1 1 d . . .
H18A H 0.4529 0.7796 0.5803 0.061 Uiso 1 1 calc R . .
H18B H 0.4635 0.6966 0.5317 0.061 Uiso 1 1 calc R . .
H18C H 0.4987 0.6932 0.6381 0.061 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'
Ga Ga 0.2307 1.6083 '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
_geom_angle_publ_flag
N2 Ga1 N1 85.90(10) . . ?
N2 Ga1 I1 118.99(8) . . ?
N1 Ga1 I1 115.85(7) . . ?
N2 Ga1 I2 123.56(8) . . ?
N1 Ga1 I2 102.66(8) . . ?
I1 Ga1 I2 106.94(2) . . ?
C5 N1 C1 120.7(3) . . ?
C5 N1 Ga1 112.6(2) . . ?
C1 N1 Ga1 126.6(2) . . ?
C7 N2 C6 119.4(2) . . ?
C7 N2 Ga1 121.75(18) . . ?
C6 N2 Ga1 115.52(18) . . ?
N1 C1 C2 121.8(3) . . ?
C1 C2 C3 118.0(3) . . ?
C4 C3 C2 120.2(3) . . ?
C3 C4 C5 119.2(3) . . ?
N1 C5 C4 120.0(3) . . ?
N1 C5 C6 116.7(2) . . ?
C4 C5 C6 123.2(3) . . ?
N2 C6 C5 109.3(2) . . ?
N2 C6 C6 113.6(3) . 2_656 ?
C5 C6 C6 112.08(16) . 2_656 ?
C8 C7 C12 119.5(3) . . ?
C8 C7 N2 118.9(3) . . ?
C12 C7 N2 121.4(3) . . ?
C9 C8 C7 119.2(3) . . ?
C9 C8 C13 117.7(3) . . ?
C7 C8 C13 123.1(3) . . ?
C10 C9 C8 121.2(3) . . ?
C9 C10 C11 119.4(3) . . ?
C10 C11 C12 122.2(4) . . ?
C11 C12 C7 118.0(3) . . ?
C11 C12 C16 117.8(3) . . ?
C7 C12 C16 124.1(3) . . ?
C8 C13 C14 112.9(3) . . ?
C8 C13 C15 111.2(3) . . ?
C14 C13 C15 110.9(4) . . ?
C12 C16 C18 111.8(3) . . ?
C12 C16 C17 111.2(3) . . ?
C18 C16 C17 109.8(3) . . ?
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
I1 Ga1 2.5092(13) . ?
I2 Ga1 2.5485(5) . ?
Ga1 N2 1.869(2) . ?
Ga1 N1 1.974(3) . ?
N1 C5 1.343(4) . ?
N1 C1 1.348(4) . ?
N2 C7 1.438(4) . ?
N2 C6 1.462(3) . ?
C1 C2 1.367(5) . ?
C2 C3 1.391(5) . ?
C3 C4 1.378(5) . ?
C4 C5 1.386(4) . ?
C5 C6 1.526(4) . ?
C6 C6 1.603(5) 2_656 ?
C7 C8 1.411(4) . ?
C7 C12 1.419(4) . ?
C8 C9 1.398(5) . ?
C8 C13 1.515(5) . ?
C9 C10 1.371(6) . ?
C10 C11 1.379(5) . ?
C11 C12 1.391(5) . ?
C12 C16 1.517(4) . ?
C13 C14 1.532(5) . ?
C13 C15 1.540(5) . ?
C16 C18 1.525(5) . ?
C16 C17 1.537(4) . ?
