#------------------------------------------------------------------------------
#$Date: 2016-08-07 11:54:08 +0300 (Sun, 07 Aug 2016) $
#$Revision: 185372 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/93/7039318.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_7039318
loop_
_publ_author_name
'Vrána, Jan'
'Ketkov, Sergey'
'Jambor, Roman'
'R°užička, Aleš'
'Lyčka, Antonín'
'Dostál, Libor'
_publ_section_title
;
 Germylenes and stannylenes stabilized within N2PE rings (E = Ge or Sn):
 combined experimental and theoretical study.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10343
_journal_page_last               10354
_journal_paper_doi               10.1039/c6dt01616b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C48 H68 Ge N4 P2'
_chemical_formula_sum            'C48 H68 Ge N4 P2'
_chemical_formula_weight         835.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-02-02 deposited with the CCDC.
2016-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1732(4)
_cell_length_b                   20.1215(8)
_cell_length_c                   15.3980(4)
_cell_measurement_reflns_used    21770
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     4701.1(3)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_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  0.0917
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21691
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.65
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.804
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.157
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         5355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0469
_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)+(0.0206P)²+6.9979P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                4475
_reflns_number_total             5355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt01616b2.cif
_cod_data_source_block           14
_cod_depositor_comments
'Adding full bibliography for 7039310--7039320.cif.'
_cod_database_code               7039318
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, 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'
'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
Ge1 Ge 0.5000 0.17190(2) 0.2500 0.02359(11) Uani 1 2 d S
P1 P 0.37208(5) 0.23587(4) 0.14672(5) 0.02414(18) Uani 1 1 d .
N1 N 0.47957(14) 0.23471(12) 0.14870(16) 0.0231(5) Uani 1 1 d .
N2 N 0.35805(15) 0.20252(11) 0.2397(2) 0.0233(5) Uani 1 1 d .
C14 C 0.25513(19) 0.10918(15) 0.2478(3) 0.0341(7) Uani 1 1 d .
C2 C 0.5273(2) 0.3282(2) 0.0569(2) 0.0329(7) Uani 1 1 d .
C13 C 0.27534(18) 0.17529(17) 0.2661(2) 0.0280(7) Uani 1 1 d .
C18 C 0.2170(2) 0.21593(19) 0.3143(2) 0.0355(8) Uani 1 1 d .
C1 C 0.52770(19) 0.25954(18) 0.0762(2) 0.0286(7) Uani 1 1 d .
C22 C 0.2403(2) 0.28646(19) 0.3357(2) 0.0384(9) Uani 1 1 d .
H22 H 0.3048 0.2886 0.3384 0.046 Uiso 1 1 d R
C10 C 0.5791(3) 0.1411(2) 0.0434(3) 0.0439(10) Uani 1 1 d .
H10 H 0.5783 0.1381 0.1069 0.053 Uiso 1 1 d R
C3 C 0.5666(3) 0.3479(2) -0.0212(3) 0.0453(11) Uani 1 1 d .
H3 H 0.5656 0.3927 -0.0357 0.054 Uiso 1 1 d R
C19 C 0.3182(3) 0.06356(17) 0.1989(3) 0.0400(9) Uani 1 1 d .
H19 H 0.3667 0.0913 0.1774 0.048 Uiso 1 1 d R
C6 C 0.5735(2) 0.2140(2) 0.0217(2) 0.0373(9) Uani 1 1 d .
C7 C 0.4863(3) 0.37927(16) 0.1160(2) 0.0374(9) Uani 1 1 d .
H7 H 0.4699 0.3568 0.1700 0.045 Uiso 1 1 d R
C15 C 0.1736(3) 0.0845(2) 0.2747(3) 0.0495(12) Uani 1 1 d .
H15 H 0.1587 0.0408 0.2620 0.059 Uiso 1 1 d R
C24 C 0.2109(3) 0.3344(2) 0.2650(3) 0.0548(11) Uani 1 1 d .
H24A H 0.2413 0.3238 0.2121 0.066 Uiso 1 1 d R
H24B H 0.2245 0.3792 0.2817 0.066 Uiso 1 1 d R
H24C H 0.1486 0.3301 0.2562 0.066 Uiso 1 1 d R
C4 C 0.6056(3) 0.3046(3) -0.0761(3) 0.0624(14) Uani 1 1 d .
H4 H 0.6289 0.3197 -0.1284 0.075 Uiso 1 1 d R
C17 C 0.1357(2) 0.1873(2) 0.3394(3) 0.0508(11) Uani 1 1 d .
H17 H 0.0951 0.2127 0.3702 0.061 Uiso 1 1 d R
C21 C 0.2763(3) 0.0302(2) 0.1201(3) 0.0574(12) Uani 1 1 d .
H21A H 0.2301 0.0011 0.1393 0.069 Uiso 1 1 d R
H21B H 0.3198 0.0051 0.0889 0.069 Uiso 1 1 d R
H21C H 0.2520 0.0637 0.0826 0.069 Uiso 1 1 d R
C20 C 0.3583(3) 0.01198(19) 0.2598(4) 0.0613(13) Uani 1 1 d .
H20A H 0.3838 0.0338 0.3092 0.074 Uiso 1 1 d R
H20B H 0.4031 -0.0126 0.2296 0.074 Uiso 1 1 d R
H20C H 0.3129 -0.0179 0.2788 0.074 Uiso 1 1 d R
C9 C 0.4024(3) 0.4090(2) 0.0771(3) 0.0539(11) Uani 1 1 d .
H9A H 0.4179 0.4373 0.0293 0.065 Uiso 1 1 d R
H9B H 0.3723 0.4347 0.1206 0.065 Uiso 1 1 d R
H9C H 0.3645 0.3741 0.0571 0.065 Uiso 1 1 d R
C5 C 0.6104(3) 0.2384(3) -0.0545(3) 0.0530(11) Uani 1 1 d .
H5 H 0.6393 0.2092 -0.0917 0.064 Uiso 1 1 d R
C23 C 0.2058(3) 0.3097(3) 0.4237(3) 0.0699(16) Uani 1 1 d .
H23A H 0.1426 0.3111 0.4222 0.084 Uiso 1 1 d R
H23B H 0.2283 0.3533 0.4363 0.084 Uiso 1 1 d R
H23C H 0.2246 0.2793 0.4680 0.084 Uiso 1 1 d R
C8 C 0.5522(3) 0.4338(2) 0.1388(4) 0.0634(14) Uani 1 1 d .
H8A H 0.5713 0.4555 0.0865 0.076 Uiso 1 1 d R
H8B H 0.6022 0.4148 0.1678 0.076 Uiso 1 1 d R
H8C H 0.5244 0.4656 0.1763 0.076 Uiso 1 1 d R
C12 C 0.5006(4) 0.10252(19) 0.0110(3) 0.0614(11) Uani 1 1 d .
H12A H 0.4479 0.1214 0.0350 0.074 Uiso 1 1 d R
H12B H 0.5056 0.0570 0.0290 0.074 Uiso 1 1 d R
H12C H 0.4980 0.1046 -0.0513 0.074 Uiso 1 1 d R
C11 C 0.6652(3) 0.1081(3) 0.0137(3) 0.0592(13) Uani 1 1 d .
H11A H 0.6663 0.1056 -0.0485 0.071 Uiso 1 1 d R
H11B H 0.6693 0.0641 0.0376 0.071 Uiso 1 1 d R
H11C H 0.7142 0.1342 0.0336 0.071 Uiso 1 1 d R
C16 C 0.1158(3) 0.1228(3) 0.3191(3) 0.0581(13) Uani 1 1 d .
H16 H 0.0619 0.1051 0.3362 0.070 Uiso 1 1 d 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'
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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.186
0 -1 0 0.151
0 1 0 0.044
-1 0 0 0.063
-1 0 1 0.091
1 0 -1 0.103
1 0 1 0.181
0 0 -1 0.152
0 0 1 0.148
-1 -1 1 0.114
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
N1 Ge1 N1 103.06(14) . 4_655
N1 Ge1 N2 68.21(9) . .
N1 Ge1 N2 91.72(10) 4_655 .
N1 Ge1 N2 91.72(10) . 4_655
N1 Ge1 N2 68.20(9) 4_655 4_655
N2 Ge1 N2 148.16(12) . 4_655
N2 P1 N1 96.35(13) . .
C1 N1 P1 119.5(2) . .
C1 N1 Ge1 137.88(19) . .
P1 N1 Ge1 100.13(12) . .
C13 N2 P1 122.3(2) . .
C13 N2 Ge1 135.8(2) . .
P1 N2 Ge1 92.92(11) . .
C13 C14 C15 118.3(4) . .
C13 C14 C19 122.4(3) . .
C15 C14 C19 119.3(3) . .
C3 C2 C1 117.1(4) . .
C3 C2 C7 120.0(4) . .
C1 C2 C7 122.8(3) . .
C14 C13 C18 121.3(3) . .
C14 C13 N2 120.1(3) . .
C18 C13 N2 118.5(3) . .
C17 C18 C13 116.9(4) . .
C17 C18 C22 122.1(4) . .
C13 C18 C22 121.0(3) . .
C2 C1 C6 120.5(3) . .
C2 C1 N1 120.4(3) . .
C6 C1 N1 119.1(3) . .
C18 C22 C24 112.0(3) . .
C18 C22 C23 113.9(4) . .
C24 C22 C23 109.9(3) . .
C18 C22 H22 106.7 . .
C24 C22 H22 107.2 . .
C23 C22 H22 106.9 . .
C6 C10 C12 112.5(4) . .
C6 C10 C11 113.8(4) . .
C12 C10 C11 110.6(4) . .
C6 C10 H10 106.3 . .
C12 C10 H10 106.8 . .
C11 C10 H10 106.3 . .
C4 C3 C2 122.8(4) . .
C4 C3 H3 118.9 . .
C2 C3 H3 118.3 . .
C20 C19 C21 110.9(3) . .
C20 C19 C14 110.8(4) . .
C21 C19 C14 113.3(3) . .
C20 C19 H19 107.2 . .
C21 C19 H19 107.1 . .
C14 C19 H19 107.2 . .
C5 C6 C1 117.8(4) . .
C5 C6 C10 120.5(4) . .
C1 C6 C10 121.6(3) . .
C2 C7 C8 111.1(4) . .
C2 C7 C9 112.0(3) . .
C8 C7 C9 110.8(3) . .
C2 C7 H7 107.6 . .
C8 C7 H7 107.7 . .
C9 C7 H7 107.5 . .
C16 C15 C14 121.5(4) . .
C16 C15 H15 119.2 . .
C14 C15 H15 119.3 . .
C22 C24 H24A 109.0 . .
C22 C24 H24B 110.0 . .
H24A C24 H24B 109.5 . .
C22 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C3 C4 C5 119.7(4) . .
C3 C4 H4 119.9 . .
C5 C4 H4 120.4 . .
C16 C17 C18 121.1(4) . .
C16 C17 H17 119.4 . .
C18 C17 H17 119.5 . .
C19 C21 H21A 109.2 . .
C19 C21 H21B 110.0 . .
H21A C21 H21B 109.5 . .
C19 C21 H21C 109.3 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C19 C20 H20A 109.7 . .
C19 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C19 C20 H20C 109.2 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C7 C9 H9A 109.1 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.8 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C4 C5 C6 121.7(4) . .
C4 C5 H5 119.1 . .
C6 C5 H5 119.2 . .
C22 C23 H23A 109.3 . .
C22 C23 H23B 109.7 . .
H23A C23 H23B 109.5 . .
C22 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C7 C8 H8A 109.3 . .
C7 C8 H8B 109.8 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.3 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C10 C12 H12A 109.1 . .
C10 C12 H12B 109.4 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.9 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.8 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.1 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C15 C16 C17 120.8(4) . .
C15 C16 H16 119.7 . .
C17 C16 H16 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 N1 2.031(3) .
Ge1 N1 2.031(3) 4_655
Ge1 N2 2.246(2) .
Ge1 N2 2.246(2) 4_655
P1 N2 1.595(3) .
P1 N1 1.632(2) .
N1 C1 1.424(4) .
N2 C13 1.428(4) .
C14 C13 1.394(5) .
C14 C15 1.396(5) .
C14 C19 1.526(5) .
C2 C3 1.399(5) .
C2 C1 1.413(5) .
C2 C7 1.507(5) .
C13 C18 1.415(5) .
C18 C17 1.415(5) .
C18 C22 1.499(6) .
C1 C6 1.423(5) .
C22 C24 1.521(5) .
C22 C23 1.527(6) .
C22 H22 0.9799 .
C10 C6 1.507(6) .
C10 C12 1.507(7) .
C10 C11 1.535(5) .
C10 H10 0.9800 .
C3 C4 1.351(7) .
C3 H3 0.9300 .
C19 C20 1.525(6) .
C19 C21 1.526(6) .
C19 H19 0.9799 .
C6 C5 1.390(5) .
C7 C8 1.525(5) .
C7 C9 1.528(5) .
C7 H7 0.9800 .
C15 C16 1.351(6) .
C15 H15 0.9300 .
C24 H24A 0.9601 .
C24 H24B 0.9599 .
C24 H24C 0.9599 .
C4 C5 1.375(7) .
C4 H4 0.9301 .
C17 C16 1.369(7) .
C17 H17 0.9300 .
C21 H21A 0.9601 .
C21 H21B 0.9600 .
C21 H21C 0.9598 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C5 H5 0.9300 .
C23 H23A 0.9599 .
C23 H23B 0.9600 .
C23 H23C 0.9601 .
C8 H8A 0.9599 .
C8 H8B 0.9601 .
C8 H8C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9601 .
C12 H12C 0.9601 .
C11 H11A 0.9601 .
C11 H11B 0.9601 .
C11 H11C 0.9600 .
C16 H16 0.9300 .
