#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:19:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180072 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/18/7051896.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_7051896
loop_
_publ_author_name
'Jin, Guoxia'
'Jones, Cameron'
'Junk, Peter C.'
'Stasch, Andreas'
'Woodul, William D.'
_publ_section_title
;
 Group 13 metal(i) and (ii) guanidinate complexes: effect of ligand
 backbone on metal oxidation state and coordination sphere
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              835
_journal_paper_doi               10.1039/b718799h
_journal_volume                  32
_journal_year                    2008
_chemical_formula_sum            'C32 H48 In N3'
_chemical_formula_weight         589.55
_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                 102.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.298(4)
_cell_length_b                   11.948(2)
_cell_length_c                   15.609(3)
_cell_measurement_temperature    150(2)
_cell_volume                     3155.0(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6276
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3340
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0394
_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)+(0.0570P)²+5.3378P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1098
_reflns_number_gt                2936
_reflns_number_total             3340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718799h.txt
_cod_data_source_block           compound14
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7051896
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
In1 In 0.5000 0.01575(2) 0.7500 0.03885(14) Uani 1 2 d S . .
N1 N 0.50004(12) 0.18408(18) 0.67874(14) 0.0222(4) Uani 1 1 d . . .
N2 N 0.5000 0.3624(3) 0.7500 0.0237(6) Uani 1 2 d S . .
C1 C 0.5000 0.2473(3) 0.7500 0.0194(7) Uani 1 2 d S . .
C2 C 0.53172(15) 0.2110(2) 0.60427(16) 0.0232(5) Uani 1 1 d . . .
C3 C 0.48118(17) 0.2053(2) 0.52132(18) 0.0281(6) Uani 1 1 d . . .
C4 C 0.5136(2) 0.2167(3) 0.44697(19) 0.0367(7) Uani 1 1 d . . .
H4 H 0.4801 0.2114 0.3906 0.044 Uiso 1 1 calc R . .
C5 C 0.5936(2) 0.2355(3) 0.4540(2) 0.0437(8) Uani 1 1 d . . .
H5 H 0.6148 0.2430 0.4029 0.052 Uiso 1 1 calc R . .
C6 C 0.64219(19) 0.2434(3) 0.5357(2) 0.0399(7) Uani 1 1 d . . .
H6 H 0.6969 0.2576 0.5402 0.048 Uiso 1 1 calc R . .
C7 C 0.61350(16) 0.2310(2) 0.61187(19) 0.0294(6) Uani 1 1 d . . .
C8 C 0.39311(17) 0.1864(3) 0.51145(19) 0.0335(6) Uani 1 1 d . . .
H8 H 0.3804 0.1951 0.5707 0.040 Uiso 1 1 calc R . .
C9 C 0.3447(2) 0.2734(4) 0.4510(3) 0.0600(11) Uani 1 1 d . . .
H9A H 0.3596 0.3487 0.4736 0.090 Uiso 1 1 calc R . .
H9B H 0.2883 0.2612 0.4488 0.090 Uiso 1 1 calc R . .
H9C H 0.3554 0.2661 0.3920 0.090 Uiso 1 1 calc R . .
C10 C 0.3697(3) 0.0690(4) 0.4799(3) 0.0730(13) Uani 1 1 d . . .
H10A H 0.3843 0.0564 0.4233 0.109 Uiso 1 1 calc R . .
H10B H 0.3125 0.0598 0.4733 0.109 Uiso 1 1 calc R . .
H10C H 0.3971 0.0147 0.5227 0.109 Uiso 1 1 calc R . .
C11 C 0.67017(16) 0.2338(3) 0.7012(2) 0.0340(6) Uani 1 1 d . . .
H11 H 0.6390 0.2565 0.7455 0.041 Uiso 1 1 calc R . .
C12 C 0.73765(19) 0.3183(3) 0.7061(3) 0.0532(9) Uani 1 1 d . . .
H12A H 0.7764 0.2890 0.6742 0.080 Uiso 1 1 calc R . .
H12B H 0.7633 0.3307 0.7675 0.080 Uiso 1 1 calc R . .
H12C H 0.7164 0.3893 0.6798 0.080 Uiso 1 1 calc R . .
C13 C 0.7037(2) 0.1172(3) 0.7260(2) 0.0503(9) Uani 1 1 d . . .
H13A H 0.6603 0.0651 0.7277 0.075 Uiso 1 1 calc R . .
H13B H 0.7392 0.1201 0.7837 0.075 Uiso 1 1 calc R . .
H13C H 0.7331 0.0916 0.6824 0.075 Uiso 1 1 calc R . .
C14 C 0.53066(15) 0.4255(2) 0.83198(17) 0.0268(6) Uani 1 1 d D . .
C15 C 0.5955(7) 0.5015(10) 0.8148(7) 0.028(3) Uani 0.50 1 d PD . .
C16 C 0.4663(6) 0.5103(9) 0.8447(7) 0.032(2) Uani 0.50 1 d PD . .
C17 C 0.5665(4) 0.5797(5) 0.7365(4) 0.0343(13) Uani 0.50 1 d PD . .
C18 C 0.6112(8) 0.4884(13) 0.8360(11) 0.046(4) Uani 0.50 1 d PD . .
C19 C 0.4685(9) 0.4877(10) 0.8724(8) 0.043(3) Uani 0.50 1 d PD . .
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'
In In -0.7276 1.3100 '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
N1 In1 N1 57.90(11) 2_656 . ?
C1 N1 C2 128.0(2) . . ?
C1 N1 In1 95.24(17) . . ?
C2 N1 In1 129.26(16) . . ?
C1 N2 C14 120.51(15) . . ?
C1 N2 C14 120.51(15) . 2_656 ?
C14 N2 C14 119.0(3) . 2_656 ?
N1 C1 N1 111.6(3) . 2_656 ?
N1 C1 N2 124.19(16) . . ?
N1 C1 N2 124.19(16) 2_656 . ?
C3 C2 C7 120.3(2) . . ?
C3 C2 N1 118.1(2) . . ?
C7 C2 N1 121.2(2) . . ?
C4 C3 C2 118.7(3) . . ?
C4 C3 C8 119.9(3) . . ?
C2 C3 C8 121.3(2) . . ?
C5 C4 C3 121.2(3) . . ?
C6 C5 C4 119.5(3) . . ?
C5 C6 C7 121.9(3) . . ?
C6 C7 C2 118.4(3) . . ?
C6 C7 C11 120.2(3) . . ?
C2 C7 C11 121.4(2) . . ?
C10 C8 C3 111.4(3) . . ?
C10 C8 C9 110.8(3) . . ?
C3 C8 C9 111.8(3) . . ?
C7 C11 C13 110.4(2) . . ?
C7 C11 C12 113.5(3) . . ?
C13 C11 C12 110.0(3) . . ?
N2 C14 C15 107.3(5) . . ?
N2 C14 C19 116.2(6) . . ?
C15 C14 C19 113.0(7) . . ?
N2 C14 C16 107.8(5) . . ?
C15 C14 C16 102.1(6) . . ?
C19 C14 C16 18.8(5) . . ?
N2 C14 C18 115.5(7) . . ?
C15 C14 C18 15.2(8) . . ?
C19 C14 C18 116.1(9) . . ?
C16 C14 C18 109.7(8) . . ?
C14 C15 C17 112.0(8) . . ?
C17 C16 C14 113.7(7) 2_656 . ?
C16 C17 C15 109.5(7) 2_656 . ?
C14 C19 C17 91.7(5) . 2_656 ?
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
In1 N1 2.298(2) 2_656 ?
In1 N1 2.298(2) . ?
N1 C1 1.345(3) . ?
N1 C2 1.421(3) . ?
N2 C1 1.375(5) . ?
N2 C14 1.484(3) . ?
N2 C14 1.484(3) 2_656 ?
C1 N1 1.345(3) 2_656 ?
C2 C3 1.405(4) . ?
C2 C7 1.415(4) . ?
C3 C4 1.396(4) . ?
C3 C8 1.516(4) . ?
C4 C5 1.384(5) . ?
C5 C6 1.377(5) . ?
C6 C7 1.388(4) . ?
C7 C11 1.528(4) . ?
C8 C10 1.514(5) . ?
C8 C9 1.530(4) . ?
C11 C13 1.528(4) . ?
C11 C12 1.533(4) . ?
C14 C15 1.510(12) . ?
C14 C19 1.546(11) . ?
C14 C16 1.549(11) . ?
C14 C18 1.573(12) . ?
C15 C17 1.537(13) . ?
C16 C17 1.522(12) 2_656 ?
C17 C16 1.522(12) 2_656 ?
C19 C17 2.009(13) 2_656 ?
