#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:43:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179344 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/41/4324153.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_4324153
loop_
_publ_author_name
'Werner Uhl'
'Thomas Abel'
'Elke Hagemeier'
'Alexander Hepp'
'Marcus Layh'
'Babak Rezaeirad'
'Heinrich Luftmann'
_publ_section_title
;
 Oligonuclear Gallium Nitrogen Cage Compounds: Molecular Intermediates on
 the Way from Gallium Hydrazides to Gallium Nitride
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              325
_journal_page_last               335
_journal_paper_doi               10.1021/ic1019839
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C16 H43 Ga4 N7'
_chemical_formula_weight         612.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   11.1768(3)
_cell_length_b                   11.1768(3)
_cell_length_c                   12.0590(6)
_cell_measurement_reflns_used    6335
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.7935
_cell_measurement_theta_min      2.6985
_cell_volume                     1304.60(8)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11138
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    4.101
_exptl_absorpt_correction_T_max  0.7910
_exptl_absorpt_correction_T_min  0.5096
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         2081
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0300
_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)+(0.0428P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0710
_reflns_number_gt                1999
_reflns_number_total             2081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1019839_si_001_7.cif
_cod_data_source_block           sad2
_cod_database_code               4324153
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, 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
Ga1 Ga 0.3333 0.6667 0.42643(4) 0.01888(14) Uani 1 3 d S . .
Ga2 Ga 0.27060(4) 0.48358(3) 0.64101(3) 0.01919(10) Uani 1 1 d . . .
N1 N 0.3333 0.6667 0.7031(4) 0.0176(9) Uani 1 3 d S . .
H1 H 0.3333 0.6667 0.7794 0.021 Uiso 1 3 calc SR . .
N11 N 0.1073(3) 0.4601(3) 0.5687(2) 0.0211(5) Uani 1 1 d . . .
N12 N 0.1594(3) 0.5958(3) 0.5120(2) 0.0205(5) Uani 1 1 d . . .
H12 H 0.0912 0.5966 0.4697 0.025 Uiso 1 1 calc R . .
C1 C 0.3333 0.6667 0.2641(5) 0.0308(14) Uani 1 3 d S . .
H1A H 0.2492 0.6599 0.2375 0.037 Uiso 0.33 1 calc PR . .
H1B H 0.3401 0.5893 0.2375 0.037 Uiso 0.33 1 calc PR . .
H1C H 0.4107 0.7508 0.2375 0.037 Uiso 0.33 1 calc PR . .
C2 C 0.2911(4) 0.3484(4) 0.7294(3) 0.0302(8) Uani 1 1 d . . .
H2A H 0.2279 0.3191 0.7908 0.036 Uiso 1 1 calc R . .
H2B H 0.3840 0.3896 0.7568 0.036 Uiso 1 1 calc R . .
H2C H 0.2714 0.2700 0.6841 0.036 Uiso 1 1 calc R . .
C12 C 0.0140(4) 0.3424(4) 0.4989(3) 0.0256(7) Uani 1 1 d . . .
C121 C 0.0780(5) 0.3317(5) 0.3897(4) 0.0500(13) Uani 1 1 d . . .
H12A H 0.0875 0.4030 0.3400 0.060 Uiso 1 1 calc R . .
H12B H 0.0194 0.2430 0.3566 0.060 Uiso 1 1 calc R . .
H12C H 0.1673 0.3423 0.4040 0.060 Uiso 1 1 calc R . .
C122 C -0.1167(5) 0.3481(5) 0.4735(5) 0.0456(11) Uani 1 1 d . . .
H12D H -0.1556 0.3581 0.5415 0.055 Uiso 1 1 calc R . .
H12E H -0.1824 0.2643 0.4371 0.055 Uiso 1 1 calc R . .
H12F H -0.0943 0.4255 0.4261 0.055 Uiso 1 1 calc R . .
C123 C -0.0270(6) 0.2140(4) 0.5678(4) 0.0460(12) Uani 1 1 d . . .
H12G H 0.0535 0.2073 0.5841 0.055 Uiso 1 1 calc R . .
H12H H -0.0921 0.1337 0.5271 0.055 Uiso 1 1 calc R . .
H12I H -0.0685 0.2196 0.6359 0.055 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'
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
C1 Ga1 N12 121.34(8) . 3_565 ?
C1 Ga1 N12 121.34(8) . . ?
N12 Ga1 N12 95.40(10) 3_565 . ?
C1 Ga1 N12 121.34(8) . 2_665 ?
N12 Ga1 N12 95.40(10) 3_565 2_665 ?
N12 Ga1 N12 95.40(10) . 2_665 ?
N11 Ga2 N1 97.83(10) . . ?
N11 Ga2 C2 127.84(15) . . ?
N1 Ga2 C2 118.82(16) . . ?
N11 Ga2 N12 98.72(11) . 2_665 ?
N1 Ga2 N12 91.89(13) . 2_665 ?
C2 Ga2 N12 114.48(14) . 2_665 ?
Ga2 N1 Ga2 106.19(14) 3_565 2_665 ?
Ga2 N1 Ga2 106.19(14) 3_565 . ?
Ga2 N1 Ga2 106.19(14) 2_665 . ?
Ga2 N1 H1 112.6 3_565 . ?
Ga2 N1 H1 112.6 2_665 . ?
Ga2 N1 H1 112.6 . . ?
C12 N11 N12 112.9(3) . . ?
C12 N11 Ga2 125.8(2) . . ?
N12 N11 Ga2 102.06(18) . . ?
N11 N12 Ga1 116.78(19) . . ?
N11 N12 Ga2 102.58(18) . 3_565 ?
Ga1 N12 Ga2 103.62(13) . 3_565 ?
N11 N12 H12 111.1 . . ?
Ga1 N12 H12 111.1 . . ?
Ga2 N12 H12 111.1 3_565 . ?
Ga1 C1 H1A 109.5 . . ?
Ga1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Ga1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Ga2 C2 H2A 109.5 . . ?
Ga2 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Ga2 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N11 C12 C123 106.0(3) . . ?
N11 C12 C122 110.1(3) . . ?
C123 C12 C122 107.9(4) . . ?
N11 C12 C121 114.4(3) . . ?
C123 C12 C121 109.2(4) . . ?
C122 C12 C121 109.0(4) . . ?
C12 C121 H12A 109.5 . . ?
C12 C121 H12B 109.5 . . ?
H12A C121 H12B 109.5 . . ?
C12 C121 H12C 109.5 . . ?
H12A C121 H12C 109.5 . . ?
H12B C121 H12C 109.5 . . ?
C12 C122 H12D 109.5 . . ?
C12 C122 H12E 109.5 . . ?
H12D C122 H12E 109.5 . . ?
C12 C122 H12F 109.5 . . ?
H12D C122 H12F 109.5 . . ?
H12E C122 H12F 109.5 . . ?
C12 C123 H12G 109.5 . . ?
C12 C123 H12H 109.5 . . ?
H12G C123 H12H 109.5 . . ?
C12 C123 H12I 109.5 . . ?
H12G C123 H12I 109.5 . . ?
H12H C123 H12I 109.5 . . ?
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
Ga1 C1 1.958(6) . ?
Ga1 N12 1.983(3) 3_565 ?
Ga1 N12 1.983(3) . ?
Ga1 N12 1.983(3) 2_665 ?
Ga2 N11 1.918(3) . ?
Ga2 N1 1.9507(18) . ?
Ga2 C2 1.954(4) . ?
Ga2 N12 2.028(3) 2_665 ?
N1 Ga2 1.9507(18) 3_565 ?
N1 Ga2 1.9507(18) 2_665 ?
N1 H1 0.9200 . ?
N11 C12 1.468(4) . ?
N11 N12 1.492(4) . ?
N12 Ga2 2.028(3) 3_565 ?
N12 H12 0.9200 . ?
C1 H1A 0.9599 . ?
C1 H1B 0.9599 . ?
C1 H1C 0.9599 . ?
C2 H2A 0.9599 . ?
C2 H2B 0.9599 . ?
C2 H2C 0.9599 . ?
C12 C123 1.518(6) . ?
C12 C122 1.524(6) . ?
C12 C121 1.532(5) . ?
C121 H12A 0.9599 . ?
C121 H12B 0.9599 . ?
C121 H12C 0.9599 . ?
C122 H12D 0.9599 . ?
C122 H12E 0.9599 . ?
C122 H12F 0.9599 . ?
C123 H12G 0.9599 . ?
C123 H12H 0.9599 . ?
C123 H12I 0.9599 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N11 Ga2 N1 Ga2 -7.54(18) . . . 3_565 ?
C2 Ga2 N1 Ga2 -149.03(18) . . . 3_565 ?
N12 Ga2 N1 Ga2 91.53(16) 2_665 . . 3_565 ?
N11 Ga2 N1 Ga2 -120.29(15) . . . 2_665 ?
C2 Ga2 N1 Ga2 98.2(2) . . . 2_665 ?
N12 Ga2 N1 Ga2 -21.22(16) 2_665 . . 2_665 ?
N1 Ga2 N11 C12 176.2(3) . . . . ?
C2 Ga2 N11 C12 -47.5(3) . . . . ?
N12 Ga2 N11 C12 83.0(3) 2_665 . . . ?
N1 Ga2 N11 N12 46.1(2) . . . . ?
C2 Ga2 N11 N12 -177.60(19) . . . . ?
N12 Ga2 N11 N12 -47.1(2) 2_665 . . . ?
C12 N11 N12 Ga1 -90.0(3) . . . . ?
Ga2 N11 N12 Ga1 47.7(2) . . . . ?
C12 N11 N12 Ga2 157.5(2) . . . 3_565 ?
Ga2 N11 N12 Ga2 -64.86(17) . . . 3_565 ?
C1 Ga1 N12 N11 107.12(19) . . . . ?
N12 Ga1 N12 N11 -120.87(15) 3_565 . . . ?
N12 Ga1 N12 N11 -24.9(2) 2_665 . . . ?
C1 Ga1 N12 Ga2 -140.96(7) . . . 3_565 ?
N12 Ga1 N12 Ga2 -8.94(12) 3_565 . . 3_565 ?
N12 Ga1 N12 Ga2 87.02(3) 2_665 . . 3_565 ?
N12 N11 C12 C123 179.1(3) . . . . ?
Ga2 N11 C12 C123 53.4(4) . . . . ?
N12 N11 C12 C122 -64.4(4) . . . . ?
Ga2 N11 C12 C122 169.9(3) . . . . ?
N12 N11 C12 C121 58.8(5) . . . . ?
Ga2 N11 C12 C121 -66.9(4) . . . . ?
