#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:23:56 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180260 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/46/7114667.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_7114667
loop_
_publ_author_name
'Hardman, Ned J.'
'Power, Philip P.'
_publ_section_title
;
 Unique structural isomerism involving tetrazole and amide/azide
 derivatives of gallium
;
_journal_issue                   13
_journal_name_full               'Chemical Communications'
_journal_page_first              1184
_journal_paper_doi               10.1039/b100466m
_journal_year                    2001
_chemical_formula_sum            'C35 H59 Ga N6 Si2'
_chemical_formula_weight         689.78
_chemical_melting_point          215
_chemical_name_common            NacNacGa(N(SiMe3)N)2
_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                 91.0640(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3462(4)
_cell_length_b                   21.9781(7)
_cell_length_c                   14.0957(4)
_cell_measurement_reflns_used    8107
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.45
_cell_measurement_theta_min      2.35
_cell_volume                     3824.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL v. 5.10'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 5.10'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 5.10'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 5.10'
_computing_structure_solution    'XS, Bruker SHELXTL v. 5.10'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.553
_diffrn_measured_fraction_theta_max 0.553
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       /w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0905
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7051
_diffrn_reflns_theta_full        31.52
_diffrn_reflns_theta_max         31.52
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        <0.01
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS: an empirical absorption program by G. M. Sheldrick

using the method described by Blessing, R. H.; Acta Cryst.

A51, 1995, 33.

;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parrallelipiped
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.45
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         7051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.117
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0442P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                4934
_reflns_number_total             7051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100466m.txt
_cod_data_source_block           nh11
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114667
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
Ga1 Ga 0.72802(2) 0.862666(9) 0.765194(18) 0.01066(7) Uani 1 1 d .
N2 N 0.58442(15) 0.89271(8) 0.72961(13) 0.0128(3) Uani 1 1 d .
Si1 Si 0.73329(6) 0.71603(3) 0.70558(5) 0.01484(12) Uani 1 1 d .
C6 C 0.48947(18) 0.85351(9) 0.72667(17) 0.0136(4) Uani 1 1 d .
C7 C 0.44258(19) 0.83383(10) 0.81124(17) 0.0171(4) Uani 1 1 d .
N3 N 0.74661(16) 0.77921(8) 0.77889(13) 0.0130(3) Uani 1 1 d .
C11 C 0.45088(18) 0.83337(9) 0.63710(17) 0.0153(4) Uani 1 1 d .
C31 C 0.6037(2) 0.67662(11) 0.7290(2) 0.0253(5) Uani 1 1 d .
H31A H 0.6032 0.6629 0.7951 0.038 Uiso 1 1 calc R
H31B H 0.5961 0.6414 0.6867 0.038 Uiso 1 1 calc R
H31C H 0.5432 0.7047 0.7175 0.038 Uiso 1 1 calc R
C32 C 0.8485(2) 0.66245(11) 0.72525(19) 0.0237(5) Uani 1 1 d .
H32A H 0.9167 0.6832 0.7117 0.036 Uiso 1 1 calc R
H32B H 0.8398 0.6273 0.6830 0.036 Uiso 1 1 calc R
H32C H 0.8495 0.6487 0.7914 0.036 Uiso 1 1 calc R
C24 C 0.79394(19) 0.91868(10) 0.46730(17) 0.0170(4) Uani 1 1 d .
H24A H 0.7352 0.9299 0.5120 0.020 Uiso 1 1 calc R
N1 N 0.80572(15) 0.91558(8) 0.67928(13) 0.0116(3) Uani 1 1 d .
C19 C 0.89179(19) 0.89612(9) 0.52503(16) 0.0147(4) Uani 1 1 d .
C12 C 0.4794(2) 0.85637(10) 0.90833(18) 0.0189(5) Uani 1 1 d .
H12A H 0.5440 0.8831 0.8999 0.023 Uiso 1 1 calc R
C27 C 1.01118(19) 0.88471(10) 0.77968(17) 0.0168(4) Uani 1 1 d .
H27A H 0.9429 0.9010 0.8070 0.020 Uiso 1 1 calc R
C18 C 0.89834(18) 0.89783(9) 0.62552(16) 0.0136(4) Uani 1 1 d .
C15 C 0.4963(2) 0.85590(10) 0.54446(18) 0.0188(5) Uani 1 1 d .
H15A H 0.5739 0.8671 0.5561 0.023 Uiso 1 1 calc R
C9 C 0.3197(2) 0.77072(10) 0.7190(2) 0.0232(5) Uani 1 1 d .
H9A H 0.2623 0.7419 0.7165 0.028 Uiso 1 1 calc R
C4 C 0.4681(2) 0.98409(10) 0.73395(19) 0.0205(5) Uani 1 1 d .
H4A H 0.4095 0.9555 0.7184 0.031 Uiso 1 1 calc R
H4B H 0.4631 1.0193 0.6915 0.031 Uiso 1 1 calc R
H4C H 0.4617 0.9976 0.7998 0.031 Uiso 1 1 calc R
C1 C 0.57564(19) 0.95311(9) 0.72170(15) 0.0134(4) Uani 1 1 d .
C2 C 0.66538(19) 0.99054(9) 0.70508(16) 0.0153(4) Uani 1 1 d .
H2A H 0.6541 1.0329 0.7136 0.018 Uiso 1 1 calc R
C3 C 0.76950(18) 0.97343(9) 0.67751(15) 0.0127(4) Uani 1 1 d .
C23 C 0.99461(19) 0.87976(10) 0.67324(17) 0.0155(4) Uani 1 1 d .
C14 C 0.5127(2) 0.80358(12) 0.97382(19) 0.0260(5) Uani 1 1 d .
H14A H 0.5725 0.7810 0.9455 0.039 Uiso 1 1 calc R
H14B H 0.4508 0.7763 0.9821 0.039 Uiso 1 1 calc R
H14C H 0.5361 0.8197 1.0357 0.039 Uiso 1 1 calc R
C16 C 0.4921(2) 0.80780(13) 0.4660(2) 0.0289(6) Uani 1 1 d .
H16A H 0.5254 0.7701 0.4893 0.043 Uiso 1 1 calc R
H16B H 0.5317 0.8225 0.4109 0.043 Uiso 1 1 calc R
H16C H 0.4165 0.8000 0.4474 0.043 Uiso 1 1 calc R
C8 C 0.3568(2) 0.79192(10) 0.80510(19) 0.0217(5) Uani 1 1 d .
H8A H 0.3240 0.7780 0.8615 0.026 Uiso 1 1 calc R
C22 C 1.0801(2) 0.85746(10) 0.62017(19) 0.0191(5) Uani 1 1 d .
H22A H 1.1444 0.8443 0.6521 0.023 Uiso 1 1 calc R
C25 C 0.7505(2) 0.87034(11) 0.39881(18) 0.0235(5) Uani 1 1 d .
H25A H 0.7347 0.8330 0.4340 0.035 Uiso 1 1 calc R
H25B H 0.8048 0.8618 0.3508 0.035 Uiso 1 1 calc R
H25C H 0.6839 0.8852 0.3677 0.035 Uiso 1 1 calc R
C21 C 1.0736(2) 0.85394(10) 0.52193(18) 0.0193(5) Uani 1 1 d .
H21A H 1.1322 0.8381 0.4869 0.023 Uiso 1 1 calc R
C20 C 0.9799(2) 0.87403(10) 0.47557(17) 0.0186(4) Uani 1 1 d .
H20A H 0.9759 0.8726 0.4082 0.022 Uiso 1 1 calc R
C30 C 0.7362(2) 0.74839(10) 0.58351(17) 0.0235(5) Uani 1 1 d .
H30A H 0.8089 0.7640 0.5710 0.035 Uiso 1 1 calc R
H30B H 0.6835 0.7816 0.5780 0.035 Uiso 1 1 calc R
H30C H 0.7177 0.7166 0.5373 0.035 Uiso 1 1 calc R
C10 C 0.3654(2) 0.79096(10) 0.63525(18) 0.0199(5) Uani 1 1 d .
H10A H 0.3386 0.7760 0.5761 0.024 Uiso 1 1 calc R
C5 C 0.8443(2) 1.02380(10) 0.6478(2) 0.0219(5) Uani 1 1 d .
H5A H 0.9115 1.0062 0.6239 0.033 Uiso 1 1 calc R
H5B H 0.8610 1.0500 0.7024 0.033 Uiso 1 1 calc R
H5C H 0.8091 1.0480 0.5976 0.033 Uiso 1 1 calc R
C13 C 0.3895(2) 0.89459(12) 0.9538(2) 0.0271(5) Uani 1 1 d .
H13A H 0.3709 0.9289 0.9122 0.041 Uiso 1 1 calc R
H13B H 0.4152 0.9100 1.0154 0.041 Uiso 1 1 calc R
H13C H 0.3253 0.8692 0.9626 0.041 Uiso 1 1 calc R
C29 C 1.0346(2) 0.82260(11) 0.82567(19) 0.0241(5) Uani 1 1 d .
H29A H 0.9765 0.7941 0.8085 0.036 Uiso 1 1 calc R
H29B H 1.0385 0.8272 0.8948 0.036 Uiso 1 1 calc R
H29C H 1.1038 0.8069 0.8030 0.036 Uiso 1 1 calc R
C17 C 0.4365(3) 0.91282(13) 0.5097(2) 0.0341(7) Uani 1 1 d .
H17A H 0.4497 0.9462 0.5545 0.051 Uiso 1 1 calc R
H17B H 0.3586 0.9044 0.5054 0.051 Uiso 1 1 calc R
H17C H 0.4628 0.9243 0.4470 0.051 Uiso 1 1 calc R
C28 C 1.1032(2) 0.92997(13) 0.8037(2) 0.0295(6) Uani 1 1 d .
H28A H 1.0863 0.9696 0.7754 0.044 Uiso 1 1 calc R
H28B H 1.1714 0.9147 0.7783 0.044 Uiso 1 1 calc R
H28C H 1.1104 0.9343 0.8727 0.044 Uiso 1 1 calc R
N6 N 0.76476(17) 0.86736(8) 0.89585(14) 0.0137(4) Uani 1 1 d .
C26 C 0.8241(2) 0.97549(11) 0.4089(2) 0.0267(6) Uani 1 1 d .
H26A H 0.8534 1.0069 0.4515 0.040 Uiso 1 1 calc R
H26B H 0.7593 0.9911 0.3758 0.040 Uiso 1 1 calc R
H26C H 0.8787 0.9645 0.3623 0.040 Uiso 1 1 calc R
Si2 Si 0.79372(6) 0.92125(3) 0.98409(5) 0.01761(14) Uani 1 1 d .
C34 C 0.7984(3) 0.99739(10) 0.92479(19) 0.0261(6) Uani 1 1 d .
H34A H 0.8559 0.9975 0.8778 0.039 Uiso 1 1 calc R
H34B H 0.8131 1.0289 0.9725 0.039 Uiso 1 1 calc R
H34C H 0.7286 1.0055 0.8931 0.039 Uiso 1 1 calc R
C35 C 0.9254(3) 0.90437(13) 1.0441(2) 0.0327(7) Uani 1 1 d .
H35A H 0.9244 0.8628 1.0692 0.049 Uiso 1 1 calc R
H35B H 0.9376 0.9332 1.0963 0.049 Uiso 1 1 calc R
H35C H 0.9839 0.9082 0.9984 0.049 Uiso 1 1 calc R
N4 N 0.76917(16) 0.76477(8) 0.87407(14) 0.0153(4) Uani 1 1 d .
N5 N 0.77953(17) 0.80829(8) 0.93223(14) 0.0164(4) Uani 1 1 d .
C33 C 0.6889(3) 0.92286(14) 1.0778(2) 0.0338(7) Uani 1 1 d .
H33A H 0.6870 0.8834 1.1099 0.051 Uiso 1 1 calc R
H33B H 0.6178 0.9313 1.0485 0.051 Uiso 1 1 calc R
H33C H 0.7068 0.9548 1.1240 0.051 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'
Si Si 0.0817 0.0704 '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
N3 Ga1 N6 85.74(7)
N3 Ga1 N1 126.41(8)
N6 Ga1 N1 117.49(8)
N3 Ga1 N2 118.11(8)
N6 Ga1 N2 115.64(8)
N1 Ga1 N2 95.40(8)
C1 N2 C6 121.45(19)
C1 N2 Ga1 115.47(15)
C6 N2 Ga1 122.38(13)
N3 Si1 C31 109.89(11)
N3 Si1 C30 103.95(10)
C31 Si1 C30 111.96(13)
N3 Si1 C32 110.68(10)
C31 Si1 C32 109.70(12)
C30 Si1 C32 110.55(13)
C7 C6 C11 121.7(2)
C7 C6 N2 120.2(2)
C11 C6 N2 118.0(2)
C8 C7 C6 118.2(2)
C8 C7 C12 118.9(2)
C6 C7 C12 123.0(2)
N4 N3 Si1 113.79(13)
N4 N3 Ga1 110.17(13)
Si1 N3 Ga1 135.83(10)
C10 C11 C6 117.7(2)
C10 C11 C15 119.3(2)
C6 C11 C15 122.98(19)
C19 C24 C25 112.13(19)
C19 C24 C26 110.5(2)
C25 C24 C26 108.1(2)
C3 N1 C18 120.87(18)
C3 N1 Ga1 114.09(15)
C18 N1 Ga1 124.93(13)
C20 C19 C18 118.7(2)
C20 C19 C24 117.7(2)
C18 C19 C24 123.6(2)
C7 C12 C14 111.6(2)
C7 C12 C13 110.3(2)
C14 C12 C13 110.4(2)
C23 C27 C29 112.0(2)
C23 C27 C28 110.4(2)
C29 C27 C28 110.4(2)
C23 C18 C19 120.0(2)
C23 C18 N1 119.7(2)
C19 C18 N1 120.18(19)
C11 C15 C17 111.1(2)
C11 C15 C16 112.9(2)
C17 C15 C16 108.9(2)
C8 C9 C10 120.6(2)
N2 C1 C2 122.2(2)
N2 C1 C4 120.7(2)
C2 C1 C4 117.06(18)
C3 C2 C1 128.34(19)
N1 C3 C2 123.6(2)
N1 C3 C5 119.6(2)
C2 C3 C5 116.77(18)
C22 C23 C18 118.8(2)
C22 C23 C27 117.9(2)
C18 C23 C27 123.3(2)
C9 C8 C7 121.1(2)
C21 C22 C23 121.7(2)
C22 C21 C20 118.9(2)
C21 C20 C19 121.8(2)
C9 C10 C11 120.8(2)
N5 N6 Si2 110.02(14)
N5 N6 Ga1 109.38(13)
Si2 N6 Ga1 140.47(10)
N6 Si2 C35 110.74(11)
N6 Si2 C33 112.36(12)
C35 Si2 C33 107.14(15)
N6 Si2 C34 107.18(10)
C35 Si2 C34 110.37(14)
C33 Si2 C34 109.06(14)
N5 N4 N3 117.72(17)
N4 N5 N6 116.80(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ga1 N3 1.8581(17)
Ga1 N6 1.8913(19)
Ga1 N1 1.9449(18)
Ga1 N2 1.9488(19)
N2 C1 1.337(3)
N2 C6 1.455(3)
Si1 N3 1.7368(19)
Si1 C31 1.854(3)
Si1 C30 1.863(2)
Si1 C32 1.863(2)
C6 C7 1.403(3)
C6 C11 1.412(3)
C7 C8 1.405(3)
C7 C12 1.517(3)
N3 N4 1.402(3)
C11 C10 1.408(3)
C11 C15 1.514(4)
C24 C19 1.527(3)
C24 C25 1.526(3)
C24 C26 1.545(3)
N1 C3 1.348(2)
N1 C18 1.437(3)
C19 C20 1.390(3)
C19 C18 1.418(3)
C12 C14 1.534(3)
C12 C13 1.541(4)
C27 C23 1.514(3)
C27 C29 1.536(3)
C27 C28 1.543(3)
C18 C23 1.412(3)
C15 C17 1.528(4)
C15 C16 1.530(3)
C9 C8 1.371(4)
C9 C10 1.390(4)
C4 C1 1.505(3)
C1 C2 1.403(3)
C2 C3 1.401(3)
C3 C5 1.506(3)
C23 C22 1.394(3)
C22 C21 1.388(4)
C21 C20 1.390(3)
N6 N5 1.406(2)
N6 Si2 1.7497(19)
Si2 C35 1.857(3)
Si2 C33 1.866(3)
Si2 C34 1.872(3)
N4 N5 1.265(3)
