#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:19:24 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180072 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/18/7051891.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_7051891
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            'C64 H96 Cl2 In2 N6'
_chemical_formula_weight         1250.01
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.02(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.518(2)
_cell_length_b                   19.205(4)
_cell_length_c                   14.668(3)
_cell_measurement_temperature    150(2)
_cell_volume                     3161.2(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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22412
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.856
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         6459
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0455
_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)+(0.0552P)²+3.3414P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                4788
_reflns_number_total             6459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718799h.txt
_cod_data_source_block           compound13
_cod_original_cell_volume        3161.0(11)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7051891
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.51462(2) 0.437997(14) 0.545120(18) 0.02629(11) Uani 1 1 d . . .
Cl1 Cl 0.44047(12) 0.33983(6) 0.45148(9) 0.0515(3) Uani 1 1 d . . .
N1 N 0.6687(3) 0.40273(17) 0.6479(2) 0.0282(7) Uani 1 1 d . . .
C1 C 0.6209(3) 0.41711(17) 0.7213(3) 0.0218(8) Uani 1 1 d . . .
N2 N 0.5062(3) 0.43601(16) 0.6916(2) 0.0256(7) Uani 1 1 d . . .
C2 C 0.7744(4) 0.3624(2) 0.8456(3) 0.0443(11) Uani 1 1 d . . .
H2 H 0.7742 0.3306 0.7916 0.053 Uiso 1 1 calc R . .
N3 N 0.6803(3) 0.41426(16) 0.8137(2) 0.0256(7) Uani 1 1 d . . .
C3 C 0.7431(5) 0.3174(3) 0.9245(3) 0.0548(13) Uani 1 1 d . . .
H3A H 0.6724 0.2882 0.8988 0.066 Uiso 1 1 calc R . .
H3B H 0.8105 0.2862 0.9515 0.066 Uiso 1 1 calc R . .
C4 C 0.7170(7) 0.3660(4) 1.0004(5) 0.099(2) Uani 1 1 d D . .
H4A H 0.7913 0.3907 1.0302 0.118 Uiso 1 1 calc R . .
H4B H 0.6928 0.3375 1.0492 0.118 Uiso 1 1 calc R . .
C5 C 0.6172(5) 0.4215(3) 0.9636(4) 0.0711(18) Uani 1 1 d D . .
H5A H 0.5395 0.3977 0.9425 0.085 Uiso 1 1 calc R . .
H5B H 0.6111 0.4538 1.0148 0.085 Uiso 1 1 calc R . .
C6 C 0.6467(4) 0.4627(2) 0.8816(3) 0.0406(11) Uani 1 1 d . . .
H6 H 0.5734 0.4883 0.8492 0.049 Uiso 1 1 calc R . .
C7 C 0.8992(4) 0.3900(4) 0.8772(5) 0.085(2) Uani 1 1 d . . .
H7A H 0.9214 0.4152 0.8256 0.127 Uiso 1 1 calc R . .
H7B H 0.9544 0.3511 0.8963 0.127 Uiso 1 1 calc R . .
H7C H 0.9033 0.4215 0.9303 0.127 Uiso 1 1 calc R . .
C8 C 0.7465(5) 0.5162(3) 0.9138(4) 0.0569(14) Uani 1 1 d . . .
H8A H 0.8193 0.4921 0.9460 0.085 Uiso 1 1 calc R . .
H8B H 0.7224 0.5495 0.9568 0.085 Uiso 1 1 calc R . .
H8C H 0.7616 0.5411 0.8593 0.085 Uiso 1 1 calc R . .
C9 C 0.7889(3) 0.3892(2) 0.6433(3) 0.0265(8) Uani 1 1 d . . .
C10 C 0.8200(4) 0.3196(2) 0.6272(3) 0.0314(9) Uani 1 1 d . . .
C11 C 0.9351(4) 0.3065(2) 0.6148(3) 0.0368(10) Uani 1 1 d . . .
H11 H 0.9580 0.2600 0.6057 0.044 Uiso 1 1 calc R . .
C12 C 1.0156(4) 0.3593(2) 0.6155(3) 0.0425(11) Uani 1 1 d . . .
H12 H 1.0931 0.3490 0.6068 0.051 Uiso 1 1 calc R . .
C13 C 0.9844(4) 0.4274(2) 0.6289(4) 0.0440(11) Uani 1 1 d . . .
H13 H 1.0405 0.4636 0.6285 0.053 Uiso 1 1 calc R . .
C14 C 0.8710(4) 0.4437(2) 0.6429(3) 0.0353(10) Uani 1 1 d . . .
C15 C 0.7328(4) 0.2604(2) 0.6222(3) 0.0442(11) Uani 1 1 d . . .
H15 H 0.6562 0.2796 0.6328 0.053 Uiso 1 1 calc R . .
C16 C 0.7073(5) 0.2243(3) 0.5280(4) 0.0585(14) Uani 1 1 d . . .
H16A H 0.6815 0.2587 0.4783 0.088 Uiso 1 1 calc R . .
H16B H 0.6442 0.1896 0.5256 0.088 Uiso 1 1 calc R . .
H16C H 0.7797 0.2011 0.5192 0.088 Uiso 1 1 calc R . .
C17 C 0.7784(6) 0.2047(3) 0.6976(4) 0.0695(17) Uani 1 1 d . . .
H17A H 0.7137 0.1722 0.7005 0.104 Uiso 1 1 calc R . .
H17B H 0.8057 0.2273 0.7585 0.104 Uiso 1 1 calc R . .
H17C H 0.8447 0.1791 0.6815 0.104 Uiso 1 1 calc R . .
C18 C 0.8406(4) 0.5201(2) 0.6545(4) 0.0448(12) Uani 1 1 d . . .
H18 H 0.7616 0.5223 0.6719 0.054 Uiso 1 1 calc R . .
C19 C 0.9315(5) 0.5561(3) 0.7300(5) 0.0673(17) Uani 1 1 d . . .
H19A H 0.9399 0.5307 0.7890 0.101 Uiso 1 1 calc R . .
H19B H 0.9052 0.6038 0.7379 0.101 Uiso 1 1 calc R . .
H19C H 1.0084 0.5573 0.7120 0.101 Uiso 1 1 calc R . .
C20 C 0.8311(5) 0.5595(3) 0.5630(5) 0.0648(16) Uani 1 1 d . . .
H20A H 0.8133 0.6086 0.5721 0.097 Uiso 1 1 calc R . .
H20B H 0.7672 0.5393 0.5147 0.097 Uiso 1 1 calc R . .
H20C H 0.9068 0.5560 0.5433 0.097 Uiso 1 1 calc R . .
C21 C 0.4129(3) 0.4348(2) 0.7424(3) 0.0255(8) Uani 1 1 d . . .
C22 C 0.3743(4) 0.3715(2) 0.7748(3) 0.0320(9) Uani 1 1 d . . .
C23 C 0.2793(4) 0.3735(2) 0.8188(3) 0.0390(10) Uani 1 1 d . . .
H23 H 0.2521 0.3313 0.8407 0.047 Uiso 1 1 calc R . .
C24 C 0.2241(4) 0.4348(2) 0.8313(3) 0.0418(11) Uani 1 1 d . . .
H24 H 0.1607 0.4350 0.8630 0.050 Uiso 1 1 calc R . .
C25 C 0.2604(4) 0.4963(2) 0.7979(3) 0.0366(10) Uani 1 1 d . . .
H25 H 0.2205 0.5385 0.8056 0.044 Uiso 1 1 calc R . .
C26 C 0.3551(3) 0.4973(2) 0.7527(3) 0.0305(9) Uani 1 1 d . . .
C27 C 0.4282(4) 0.3013(2) 0.7583(3) 0.0400(10) Uani 1 1 d . . .
H27 H 0.5118 0.3096 0.7523 0.048 Uiso 1 1 calc R . .
C28 C 0.4324(5) 0.2498(3) 0.8388(4) 0.0661(16) Uani 1 1 d . . .
H28A H 0.4675 0.2726 0.8984 0.099 Uiso 1 1 calc R . .
H28B H 0.4809 0.2094 0.8303 0.099 Uiso 1 1 calc R . .
H28C H 0.3513 0.2344 0.8390 0.099 Uiso 1 1 calc R . .
C29 C 0.3589(5) 0.2698(3) 0.6665(4) 0.0646(15) Uani 1 1 d . . .
H29A H 0.2774 0.2591 0.6717 0.097 Uiso 1 1 calc R . .
H29B H 0.3982 0.2269 0.6534 0.097 Uiso 1 1 calc R . .
H29C H 0.3565 0.3031 0.6155 0.097 Uiso 1 1 calc R . .
C30 C 0.3889(4) 0.5659(2) 0.7130(3) 0.0379(10) Uani 1 1 d . . .
H30 H 0.4646 0.5585 0.6918 0.046 Uiso 1 1 calc R . .
C31 C 0.4092(5) 0.6247(3) 0.7855(4) 0.0649(16) Uani 1 1 d . . .
H31A H 0.4342 0.6669 0.7575 0.097 Uiso 1 1 calc R . .
H31B H 0.4714 0.6109 0.8397 0.097 Uiso 1 1 calc R . .
H31C H 0.3350 0.6340 0.8054 0.097 Uiso 1 1 calc R . .
C32 C 0.2926(5) 0.5879(3) 0.6285(4) 0.0563(13) Uani 1 1 d . . .
H32A H 0.2806 0.5508 0.5814 0.085 Uiso 1 1 calc R . .
H32B H 0.3174 0.6306 0.6017 0.085 Uiso 1 1 calc R . .
H32C H 0.2179 0.5964 0.6481 0.085 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'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 N2 61.17(12) . . ?
N1 In1 Cl1 106.62(10) . . ?
N2 In1 Cl1 117.87(9) . . ?
N1 In1 C1 30.66(11) . . ?
N2 In1 C1 30.69(11) . . ?
Cl1 In1 C1 118.32(8) . . ?
N1 In1 In1 127.46(9) . 3_666 ?
N2 In1 In1 118.06(8) . 3_666 ?
Cl1 In1 In1 115.24(4) . 3_666 ?
C1 In1 In1 126.41(8) . 3_666 ?
C1 N1 C9 130.8(3) . . ?
C1 N1 In1 94.2(2) . . ?
C9 N1 In1 132.7(2) . . ?
N1 C1 N2 110.3(3) . . ?
N1 C1 N3 125.3(3) . . ?
N2 C1 N3 124.3(3) . . ?
N1 C1 In1 55.13(18) . . ?
N2 C1 In1 55.59(19) . . ?
N3 C1 In1 173.3(3) . . ?
C1 N2 C21 128.5(3) . . ?
C1 N2 In1 93.7(2) . . ?
C21 N2 In1 135.8(2) . . ?
N3 C2 C7 116.4(4) . . ?
N3 C2 C3 109.7(4) . . ?
C7 C2 C3 109.5(4) . . ?
C1 N3 C2 120.6(3) . . ?
C1 N3 C6 119.4(3) . . ?
C2 N3 C6 119.9(3) . . ?
C4 C3 C2 108.6(5) . . ?
C3 C4 C5 114.2(5) . . ?
C6 C5 C4 110.1(5) . . ?
N3 C6 C8 109.7(4) . . ?
N3 C6 C5 109.8(4) . . ?
C8 C6 C5 112.7(4) . . ?
C14 C9 C10 120.3(3) . . ?
C14 C9 N1 121.6(3) . . ?
C10 C9 N1 117.7(3) . . ?
C11 C10 C9 118.2(4) . . ?
C11 C10 C15 119.9(4) . . ?
C9 C10 C15 121.9(4) . . ?
C12 C11 C10 121.6(4) . . ?
C11 C12 C13 120.2(4) . . ?
C12 C13 C14 120.9(4) . . ?
C13 C14 C9 118.8(4) . . ?
C13 C14 C18 118.4(4) . . ?
C9 C14 C18 122.8(4) . . ?
C10 C15 C16 112.3(4) . . ?
C10 C15 C17 111.9(4) . . ?
C16 C15 C17 107.5(4) . . ?
C19 C18 C20 108.6(4) . . ?
C19 C18 C14 112.6(4) . . ?
C20 C18 C14 110.6(4) . . ?
C26 C21 C22 120.6(4) . . ?
C26 C21 N2 118.2(3) . . ?
C22 C21 N2 121.1(3) . . ?
C23 C22 C21 118.2(4) . . ?
C23 C22 C27 119.2(4) . . ?
C21 C22 C27 122.5(4) . . ?
C24 C23 C22 121.6(4) . . ?
C23 C24 C25 120.1(4) . . ?
C24 C25 C26 120.8(4) . . ?
C21 C26 C25 118.7(4) . . ?
C21 C26 C30 122.1(3) . . ?
C25 C26 C30 119.1(4) . . ?
C22 C27 C29 109.8(4) . . ?
C22 C27 C28 113.1(4) . . ?
C29 C27 C28 110.0(4) . . ?
C32 C30 C26 110.4(4) . . ?
C32 C30 C31 109.2(4) . . ?
C26 C30 C31 112.6(4) . . ?
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 2.162(3) . ?
In1 N2 2.173(3) . ?
In1 Cl1 2.3752(12) . ?
In1 C1 2.628(4) . ?
In1 In1 2.7085(7) 3_666 ?
N1 C1 1.344(5) . ?
N1 C9 1.425(5) . ?
C1 N2 1.344(5) . ?
C1 N3 1.375(5) . ?
N2 C21 1.439(5) . ?
C2 N3 1.468(5) . ?
C2 C7 1.504(7) . ?
C2 C3 1.550(6) . ?
N3 C6 1.477(5) . ?
C3 C4 1.535(8) . ?
C4 C5 1.570(4) . ?
C5 C6 1.541(7) . ?
C6 C8 1.534(7) . ?
C9 C14 1.412(6) . ?
C9 C10 1.417(5) . ?
C10 C11 1.401(5) . ?
C10 C15 1.509(6) . ?
C11 C12 1.372(6) . ?
C12 C13 1.382(6) . ?
C13 C14 1.402(6) . ?
C14 C18 1.527(6) . ?
C15 C16 1.515(6) . ?
C15 C17 1.543(7) . ?
C18 C19 1.509(7) . ?
C18 C20 1.524(7) . ?
C21 C26 1.398(5) . ?
C21 C22 1.413(5) . ?
C22 C23 1.391(6) . ?
C22 C27 1.525(6) . ?
C23 C24 1.371(6) . ?
C24 C25 1.379(6) . ?
C25 C26 1.398(5) . ?
C26 C30 1.526(6) . ?
C27 C29 1.528(7) . ?
C27 C28 1.532(6) . ?
C30 C32 1.525(7) . ?
C30 C31 1.532(6) . ?
