#------------------------------------------------------------------------------
#$Date: 2016-03-26 15:01:28 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180284 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/70/7117028.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_7117028
loop_
_publ_author_name
'Benjamin Peerless'
'Theo Keane'
'Anthony J. H. M. Meijer'
'Peter Portius'
_publ_section_title
;
 Homoleptic low-valent polyazides of group 14 elements
;
_journal_name_full               Chem.Commun.
_journal_page_first              7435
_journal_paper_doi               10.1039/C5cc00259A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C24 H20 P, Ge N9'
_chemical_formula_sum            'C24 H20 Ge N9 P'
_chemical_formula_weight         538.07
_chemical_name_common            (PPh4)[Ge(N3)3]
_chemical_name_systematic        (PPh4)[Ge(N3)3]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-10-18 deposited with the CCDC.
2015-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                93.278(2)
_cell_angle_beta                 99.357(2)
_cell_angle_gamma                100.865(2)
_cell_formula_units_Z            2
_cell_length_a                   7.7712(2)
_cell_length_b                   11.4711(4)
_cell_length_c                   14.2003(4)
_cell_measurement_reflns_used    4545
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.4081
_cell_measurement_theta_min      2.4303
_cell_volume                     1221.59(6)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows'
_computing_publication_material  'ORTEP-3 for Windows'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24413
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         1.815
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.351
_exptl_absorpt_correction_T_max  0.9233
_exptl_absorpt_correction_T_min  0.7117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_description       needle
_exptl_crystal_F_000             548
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0319P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0807
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4124
_reflns_number_total             5613
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc00259a2.cif
_cod_data_source_block           ch1ppx202_0m
_cod_database_code               7117028
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.712
_shelx_estimated_absorpt_t_max   0.923
_shelxl_version_number           2014-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.47171(3) 0.29007(2) 0.68416(2) 0.02765(9) Uani 1 1 d . . . . .
N1 N 0.5845(3) 0.37359(19) 0.58397(15) 0.0365(5) Uani 1 1 d . . . . .
N2 N 0.6861(3) 0.3245(2) 0.54775(14) 0.0337(5) Uani 1 1 d . . . . .
N3 N 0.7808(3) 0.2800(2) 0.51064(16) 0.0489(7) Uani 1 1 d . . . . .
N4 N 0.6713(3) 0.3758(2) 0.78702(16) 0.0387(6) Uani 1 1 d . . . . .
N5 N 0.6515(3) 0.37344(18) 0.86967(16) 0.0299(5) Uani 1 1 d . . . . .
N6 N 0.6393(3) 0.3735(2) 0.94887(16) 0.0455(6) Uani 1 1 d . . . . .
N7 N 0.5808(3) 0.14890(18) 0.66729(14) 0.0302(5) Uani 1 1 d . . . . .
N8 N 0.7244(3) 0.14444(18) 0.71238(15) 0.0326(5) Uani 1 1 d . . . . .
N9 N 0.8565(3) 0.1319(2) 0.75448(19) 0.0589(8) Uani 1 1 d . . . . .
P1 P 0.54012(8) 0.77428(5) 0.76571(4) 0.02009(14) Uani 1 1 d . . . . .
C1 C 0.6533(3) 0.7889(2) 0.66530(15) 0.0208(5) Uani 1 1 d . . . . .
C2 C 0.7692(3) 0.7114(2) 0.65349(16) 0.0252(5) Uani 1 1 d . . . . .
H2 H 0.7782 0.6493 0.6944 0.030 Uiso 1 1 calc R U . . .
C3 C 0.8704(3) 0.7260(2) 0.58192(16) 0.0280(6) Uani 1 1 d . . . . .
H3 H 0.9486 0.6734 0.5731 0.034 Uiso 1 1 calc R U . . .
C4 C 0.8581(3) 0.8171(2) 0.52305(16) 0.0297(6) Uani 1 1 d . . . . .
H4 H 0.9304 0.8281 0.4751 0.036 Uiso 1 1 calc R U . . .
C5 C 0.7419(3) 0.8923(2) 0.53330(16) 0.0297(6) Uani 1 1 d . . . . .
H5 H 0.7324 0.9534 0.4914 0.036 Uiso 1 1 calc R U . . .
C6 C 0.6387(3) 0.8789(2) 0.60476(16) 0.0249(5) Uani 1 1 d . . . . .
H6 H 0.5590 0.9308 0.6121 0.030 Uiso 1 1 calc R U . . .
C7 C 0.4397(3) 0.8996(2) 0.78618(16) 0.0206(5) Uani 1 1 d . . . . .
C8 C 0.2832(3) 0.9071(2) 0.72465(16) 0.0245(5) Uani 1 1 d . . . . .
H8 H 0.2372 0.8495 0.6714 0.029 Uiso 1 1 calc R U . . .
C9 C 0.1956(3) 0.9979(2) 0.74118(17) 0.0282(6) Uani 1 1 d . . . . .
H9 H 0.0894 1.0029 0.6991 0.034 Uiso 1 1 calc R U . . .
C10 C 0.2617(3) 1.0819(2) 0.81890(17) 0.0301(6) Uani 1 1 d . . . . .
H10 H 0.2002 1.1439 0.8303 0.036 Uiso 1 1 calc R U . . .
C11 C 0.4173(3) 1.0758(2) 0.87998(17) 0.0285(6) Uani 1 1 d . . . . .
H11 H 0.4630 1.1342 0.9327 0.034 Uiso 1 1 calc R U . . .
C12 C 0.5064(3) 0.9845(2) 0.86427(16) 0.0250(5) Uani 1 1 d . . . . .
H12 H 0.6124 0.9798 0.9066 0.030 Uiso 1 1 calc R U . . .
C13 C 0.7064(3) 0.7630(2) 0.86687(16) 0.0235(5) Uani 1 1 d . . . . .
C14 C 0.8666(3) 0.8460(2) 0.88210(17) 0.0311(6) Uani 1 1 d . . . . .
H14 H 0.8851 0.9075 0.8406 0.037 Uiso 1 1 calc R U . . .
C15 C 0.9981(3) 0.8377(3) 0.95825(19) 0.0389(7) Uani 1 1 d . . . . .
H15 H 1.1077 0.8937 0.9691 0.047 Uiso 1 1 calc R U . . .
C16 C 0.9710(4) 0.7485(3) 1.01846(18) 0.0394(7) Uani 1 1 d . . . . .
H16 H 1.0617 0.7437 1.0708 0.047 Uiso 1 1 calc R U . . .
C17 C 0.8130(4) 0.6663(3) 1.00308(18) 0.0377(7) Uani 1 1 d . . . . .
H17 H 0.7955 0.6048 1.0446 0.045 Uiso 1 1 calc R U . . .
C18 C 0.6795(3) 0.6732(2) 0.92706(16) 0.0294(6) Uani 1 1 d . . . . .
H18 H 0.5703 0.6167 0.9164 0.035 Uiso 1 1 calc R U . . .
C19 C 0.3607(3) 0.6476(2) 0.74614(15) 0.0211(5) Uani 1 1 d . . . . .
C20 C 0.3290(3) 0.5673(2) 0.66522(16) 0.0248(5) Uani 1 1 d . . . . .
H20 H 0.4094 0.5744 0.6211 0.030 Uiso 1 1 calc R U . . .
C21 C 0.1796(3) 0.4771(2) 0.64957(18) 0.0310(6) Uani 1 1 d . . . . .
H21 H 0.1571 0.4224 0.5941 0.037 Uiso 1 1 calc R U . . .
C22 C 0.0627(3) 0.4652(2) 0.71323(18) 0.0327(6) Uani 1 1 d . . . . .
H22 H -0.0400 0.4030 0.7013 0.039 Uiso 1 1 calc R U . . .
C23 C 0.0950(3) 0.5439(2) 0.79452(18) 0.0304(6) Uani 1 1 d . . . . .
H23 H 0.0155 0.5345 0.8391 0.036 Uiso 1 1 calc R U . . .
C24 C 0.2412(3) 0.6354(2) 0.81121(16) 0.0257(5) Uani 1 1 d . . . . .
H24 H 0.2616 0.6903 0.8664 0.031 Uiso 1 1 calc R U . . .
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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
N7 Ge1 N1 93.50(9) . .
N7 Ge1 N4 94.37(9) . .
N1 Ge1 N4 90.98(9) . .
N2 N1 Ge1 116.40(17) . .
N3 N2 N1 177.6(3) . .
N5 N4 Ge1 118.61(17) . .
N6 N5 N4 177.4(3) . .
N8 N7 Ge1 121.20(17) . .
N9 N8 N7 175.3(3) . .
C19 P1 C1 111.75(10) . .
C19 P1 C7 105.22(10) . .
C1 P1 C7 111.57(11) . .
C19 P1 C13 111.77(11) . .
C1 P1 C13 105.91(10) . .
C7 P1 C13 110.74(10) . .
C6 C1 C2 120.2(2) . .
C6 C1 P1 122.02(17) . .
C2 C1 P1 117.57(17) . .
C3 C2 C1 119.5(2) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
C2 C3 C4 120.1(2) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C5 C4 C3 120.6(2) . .
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
C4 C5 C6 120.1(2) . .
C4 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C1 C6 C5 119.4(2) . .
C1 C6 H6 120.3 . .
C5 C6 H6 120.3 . .
C12 C7 C8 119.6(2) . .
C12 C7 P1 122.16(18) . .
C8 C7 P1 118.08(17) . .
C9 C8 C7 120.1(2) . .
C9 C8 H8 120.0 . .
C7 C8 H8 120.0 . .
C8 C9 C10 120.2(2) . .
C8 C9 H9 119.9 . .
C10 C9 H9 119.9 . .
C11 C10 C9 120.2(2) . .
C11 C10 H10 119.9 . .
C9 C10 H10 119.9 . .
C10 C11 C12 120.1(2) . .
C10 C11 H11 120.0 . .
C12 C11 H11 120.0 . .
C11 C12 C7 119.8(2) . .
C11 C12 H12 120.1 . .
C7 C12 H12 120.1 . .
C18 C13 C14 120.4(2) . .
C18 C13 P1 121.45(18) . .
C14 C13 P1 118.13(19) . .
C15 C14 C13 119.2(3) . .
C15 C14 H14 120.4 . .
C13 C14 H14 120.4 . .
C16 C15 C14 120.4(3) . .
C16 C15 H15 119.8 . .
C14 C15 H15 119.8 . .
C15 C16 C17 120.3(2) . .
C15 C16 H16 119.8 . .
C17 C16 H16 119.8 . .
C16 C17 C18 120.1(3) . .
C16 C17 H17 119.9 . .
C18 C17 H17 119.9 . .
C13 C18 C17 119.5(2) . .
C13 C18 H18 120.2 . .
C17 C18 H18 120.2 . .
C20 C19 C24 119.7(2) . .
C20 C19 P1 121.83(18) . .
C24 C19 P1 118.27(17) . .
C21 C20 C19 119.3(2) . .
C21 C20 H20 120.3 . .
C19 C20 H20 120.3 . .
C22 C21 C20 120.9(2) . .
C22 C21 H21 119.5 . .
C20 C21 H21 119.5 . .
C21 C22 C23 119.9(2) . .
C21 C22 H22 120.0 . .
C23 C22 H22 120.0 . .
C24 C23 C22 120.3(2) . .
C24 C23 H23 119.8 . .
C22 C23 H23 119.8 . .
C23 C24 C19 119.7(2) . .
C23 C24 H24 120.1 . .
C19 C24 H24 120.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 N7 1.984(2) .
Ge1 N1 1.989(2) .
Ge1 N4 2.007(2) .
N1 N2 1.213(3) .
N2 N3 1.148(3) .
N4 N5 1.209(3) .
N5 N6 1.144(3) .
N7 N8 1.204(3) .
N8 N9 1.139(3) .
P1 C19 1.788(2) .
P1 C1 1.793(2) .
P1 C7 1.791(2) .
P1 C13 1.797(2) .
C1 C6 1.390(3) .
C1 C2 1.402(3) .
C2 C3 1.382(3) .
C2 H2 0.9500 .
C3 C4 1.383(3) .
C3 H3 0.9500 .
C4 C5 1.379(3) .
C4 H4 0.9500 .
C5 C6 1.390(3) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C12 1.395(3) .
C7 C8 1.398(3) .
C8 C9 1.376(3) .
C8 H8 0.9500 .
C9 C10 1.385(3) .
C9 H9 0.9500 .
C10 C11 1.384(3) .
C10 H10 0.9500 .
C11 C12 1.386(3) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C18 1.383(3) .
C13 C14 1.395(3) .
C14 C15 1.383(3) .
C14 H14 0.9500 .
C15 C16 1.378(4) .
C15 H15 0.9500 .
C16 C17 1.377(4) .
C16 H16 0.9500 .
C17 C18 1.388(3) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 C20 1.390(3) .
C19 C24 1.407(3) .
C20 C21 1.380(3) .
C20 H20 0.9500 .
C21 C22 1.377(3) .
C21 H21 0.9500 .
C22 C23 1.382(3) .
C22 H22 0.9500 .
C23 C24 1.373(3) .
C23 H23 0.9500 .
C24 H24 0.9500 .
