#------------------------------------------------------------------------------
#$Date: 2020-12-31 01:57:27 +0200 (Thu, 31 Dec 2020) $
#$Revision: 260254 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/54/4135437.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_4135437
loop_
_publ_author_name
'Sharma, Mahendra K.'
'Ebeler, Falk'
'Glodde, Timo'
'Neumann, Beate'
'Stammler, Hans-Georg'
'Ghadwal, Rajendra S.'
_publ_section_title
;
 Isolation of a Ge(I) Diradicaloid and Dihydrogen Splitting.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11828
_journal_year                    2020
_chemical_formula_moiety         'C78 H88 Ge2 N4 S2, 1.5(C6 H6)'
_chemical_formula_sum            'C87 H97 Ge2 N4 S2'
_chemical_formula_weight         1407.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-04
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_cell_angle_alpha                101.491(3)
_cell_angle_beta                 101.127(2)
_cell_angle_gamma                100.578(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0725(3)
_cell_length_b                   16.4856(6)
_cell_length_c                   22.3612(7)
_cell_measurement_reflns_used    13705
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.4750
_cell_measurement_theta_min      2.2100
_cell_volume                     3818.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     -4.00  40.00   1.00   72.00    --   24.86  77.00 120.00   44
  2  ω     36.00  89.00   1.00   72.00    --   24.86  57.00  90.00   53
  3  ω     -4.00  41.00   1.00   72.00    --   24.86  77.00 -30.00   45
  4  ω    -40.00  43.00   1.00   72.00    --   24.86 -57.00-150.00   83
  5  ω    -45.00  40.00   1.00   72.00    --   24.86 -38.00  90.00   85
  6  ω      3.00  37.00   1.00   72.00    --   24.86  77.00-150.00   34
  7  ω    -42.00  53.00   1.00   72.00    --   24.86 -77.00   0.00   95
  8  ω    -29.00  -3.00   1.00   72.00    --   24.86 -38.00 -60.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0103169000
_diffrn_orient_matrix_UB_12      0.0308196000
_diffrn_orient_matrix_UB_13      -0.0176566000
_diffrn_orient_matrix_UB_21      -0.0656227000
_diffrn_orient_matrix_UB_22      -0.0103244000
_diffrn_orient_matrix_UB_23      -0.0144059000
_diffrn_orient_matrix_UB_31      -0.0094674000
_diffrn_orient_matrix_UB_32      0.0313018000
_diffrn_orient_matrix_UB_33      0.0243215000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44605
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.267
_diffrn_reflns_theta_min         1.788
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.888
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.488
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1486
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         24015
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0460
_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)+(0.0267P)²+3.0456P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18216
_reflns_number_total             24015
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c11828_si_004.cif
_cod_data_source_block           compound4
_cod_database_code               4135437
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C87H97Ge2N4S2
_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_max   0.942
_shelx_estimated_absorpt_t_min   0.698
_diffrn_oxdiff_digest_frames
;
016a4f04332918792ff8fe65567d69406d00469aca4
;
_diffrn_oxdiff_digest_hkl
;
011fb90f7f0725345c7768ffb0ed66cd5a0231
;
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C43(H43), C46(H46), C55(H55), C58(H58)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C31(H31), C32(H32),
 C33(H33), C34(H34), C35(H35), C39(H39), C40(H40), C41(H41), C51(H51), C52(H52),
  C53(H53), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C68(H68),
 C69(H69), C70(H70), C71(H71), C72(H72), C74(H74), C75(H75), C76(H76), C77(H77),
  C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
 C85(H85), C86(H86), C87(H87)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C59(H59A,H59B,
 H59C), C60(H60A,H60B,H60C)
;
_olex2_date_sample_data_collection 2020-03-03
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.231
_oxdiff_exptl_absorpt_empirical_full_min 0.808
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 0.15786(2) 0.64721(2) 0.37344(2) 0.01238(5) Uani 1 1 d . . . . .
Ge2 Ge 0.13776(2) 0.66114(2) 0.18825(2) 0.01296(5) Uani 1 1 d . . . . .
S1 S 0.37326(5) 0.71570(3) 0.39256(2) 0.01888(10) Uani 1 1 d . . . . .
S2 S 0.35423(5) 0.67019(4) 0.19789(3) 0.02285(11) Uani 1 1 d . . . . .
N1 N 0.05766(14) 0.79739(10) 0.34765(7) 0.0129(3) Uani 1 1 d . . . . .
N2 N 0.11516(14) 0.82543(10) 0.26567(7) 0.0135(3) Uani 1 1 d . . . . .
N3 N 0.13627(15) 0.47488(10) 0.29383(7) 0.0148(3) Uani 1 1 d . . . . .
N4 N 0.08172(15) 0.47805(10) 0.19625(7) 0.0153(3) Uani 1 1 d . . . . .
C1 C 0.10508(17) 0.72832(11) 0.32161(9) 0.0136(3) Uani 1 1 d . . . . .
C2 C 0.13711(17) 0.74491(11) 0.26796(8) 0.0128(3) Uani 1 1 d . . . . .
C3 C 0.14965(17) 0.56117(11) 0.29342(9) 0.0136(3) Uani 1 1 d . . . . .
C4 C 0.11904(17) 0.56348(12) 0.23130(9) 0.0141(3) Uani 1 1 d . . . . .
C5 C 0.06473(17) 0.85583(12) 0.31330(9) 0.0139(3) Uani 1 1 d . . . . .
C6 C -0.00888(18) 0.79862(12) 0.39726(9) 0.0145(3) Uani 1 1 d . . . . .
C7 C 0.05379(19) 0.84535(12) 0.45815(9) 0.0178(4) Uani 1 1 d . . . . .
C8 C -0.0174(2) 0.84838(14) 0.50333(10) 0.0224(4) Uani 1 1 d . . . . .
H8 H 0.021006 0.880843 0.545069 0.027 Uiso 1 1 calc R . . . .
C9 C -0.1424(2) 0.80519(14) 0.48859(10) 0.0247(5) Uani 1 1 d . . . . .
H9 H -0.188827 0.808250 0.520202 0.030 Uiso 1 1 calc R . . . .
C10 C -0.2008(2) 0.75742(13) 0.42821(10) 0.0221(4) Uani 1 1 d . . . . .
H10 H -0.286700 0.727387 0.419024 0.026 Uiso 1 1 calc R . . . .
C11 C -0.13559(18) 0.75272(12) 0.38064(9) 0.0157(4) Uani 1 1 d . . . . .
C12 C 0.19209(19) 0.89109(14) 0.47636(10) 0.0227(4) Uani 1 1 d . . . . .
H12 H 0.230648 0.872096 0.440619 0.027 Uiso 1 1 calc R . . . .
C13 C 0.2077(2) 0.98774(15) 0.48813(12) 0.0339(6) Uani 1 1 d . . . . .
H13A H 0.297866 1.015546 0.498690 0.051 Uiso 1 1 calc GR . . . .
H13B H 0.170452 1.007800 0.523037 0.051 Uiso 1 1 calc GR . . . .
H13C H 0.164770 1.001632 0.450174 0.051 Uiso 1 1 calc GR . . . .
C14 C 0.2630(2) 0.86837(17) 0.53439(11) 0.0320(5) Uani 1 1 d . . . . .
H14A H 0.232845 0.891812 0.571087 0.048 Uiso 1 1 calc GR . . . .
H14B H 0.353840 0.892410 0.541778 0.048 Uiso 1 1 calc GR . . . .
H14C H 0.247488 0.806369 0.527412 0.048 Uiso 1 1 calc GR . . . .
C15 C -0.19873(18) 0.69843(12) 0.31499(9) 0.0176(4) Uani 1 1 d . . . . .
H15 H -0.148814 0.718229 0.285688 0.021 Uiso 1 1 calc R . . . .
C16 C -0.3354(2) 0.70564(15) 0.29197(11) 0.0263(5) Uani 1 1 d . . . . .
H16A H -0.388372 0.681261 0.317344 0.039 Uiso 1 1 calc GR . . . .
H16B H -0.367720 0.674600 0.247800 0.039 Uiso 1 1 calc GR . . . .
H16C H -0.337297 0.765671 0.296074 0.039 Uiso 1 1 calc GR . . . .
C17 C -0.19540(19) 0.60543(13) 0.31200(10) 0.0224(4) Uani 1 1 d . . . . .
H17A H -0.238974 0.585490 0.342404 0.034 Uiso 1 1 calc GR . . . .
H17B H -0.107312 0.600493 0.322081 0.034 Uiso 1 1 calc GR . . . .
H17C H -0.237792 0.570685 0.269602 0.034 Uiso 1 1 calc GR . . . .
C18 C 0.15404(18) 0.87594(12) 0.22398(9) 0.0153(4) Uani 1 1 d . . . . .
C19 C 0.06266(18) 0.88807(12) 0.17629(9) 0.0165(4) Uani 1 1 d . . . . .
C20 C 0.1035(2) 0.94520(14) 0.14204(10) 0.0245(4) Uani 1 1 d . . . . .
H20 H 0.044249 0.954969 0.108969 0.029 Uiso 1 1 calc R . . . .
C21 C 0.2287(2) 0.98773(15) 0.15544(11) 0.0301(5) Uani 1 1 d . . . . .
H21 H 0.253853 1.028300 0.132795 0.036 Uiso 1 1 calc R . . . .
C22 C 0.3179(2) 0.97196(14) 0.20151(11) 0.0278(5) Uani 1 1 d . . . . .
H22 H 0.404152 1.000562 0.209114 0.033 Uiso 1 1 calc R . . . .
C23 C 0.28361(19) 0.91486(12) 0.23694(10) 0.0198(4) Uani 1 1 d . . . . .
C24 C -0.07488(18) 0.84037(13) 0.15947(9) 0.0181(4) Uani 1 1 d . . . . .
H24 H -0.087802 0.808211 0.192087 0.022 Uiso 1 1 calc R . . . .
C25 C -0.1658(2) 0.90007(14) 0.15825(10) 0.0250(4) Uani 1 1 d . . . . .
H25A H -0.160071 0.928643 0.124094 0.037 Uiso 1 1 calc GR . . . .
H25B H -0.142963 0.942703 0.198424 0.037 Uiso 1 1 calc GR . . . .
H25C H -0.252531 0.867053 0.151457 0.037 Uiso 1 1 calc GR . . . .
C26 C -0.1048(2) 0.77593(14) 0.09590(10) 0.0251(4) Uani 1 1 d . . . . .
H26A H -0.094212 0.806172 0.063028 0.038 Uiso 1 1 calc GR . . . .
H26B H -0.192326 0.742937 0.086413 0.038 Uiso 1 1 calc GR . . . .
H26C H -0.047171 0.737460 0.097573 0.038 Uiso 1 1 calc GR . . . .
C27 C 0.38212(19) 0.89560(13) 0.28653(11) 0.0240(4) Uani 1 1 d . . . . .
H27 H 0.352285 0.835026 0.287723 0.029 Uiso 1 1 calc R . . . .
C28 C 0.3971(2) 0.95076(17) 0.35242(12) 0.0374(6) Uani 1 1 d . . . . .
H28A H 0.424060 1.010866 0.352606 0.056 Uiso 1 1 calc GR . . . .
H28B H 0.460746 0.935619 0.382495 0.056 Uiso 1 1 calc GR . . . .
H28C H 0.315923 0.941112 0.364348 0.056 Uiso 1 1 calc GR . . . .
C29 C 0.5107(2) 0.90418(16) 0.27032(14) 0.0371(6) Uani 1 1 d . . . . .
H29A H 0.566562 0.881585 0.299049 0.056 Uiso 1 1 calc GR . . . .
H29B H 0.548085 0.964314 0.274487 0.056 Uiso 1 1 calc GR . . . .
H29C H 0.500151 0.872153 0.227007 0.056 Uiso 1 1 calc GR . . . .
C30 C 0.01846(18) 0.93484(12) 0.32216(9) 0.0159(4) Uani 1 1 d . . . . .
C31 C -0.10620(19) 0.93175(13) 0.32590(9) 0.0187(4) Uani 1 1 d . . . . .
H31 H -0.159653 0.879314 0.325328 0.022 Uiso 1 1 calc R . . . .
C32 C -0.1531(2) 1.00483(13) 0.33046(10) 0.0224(4) Uani 1 1 d . . . . .
H32 H -0.238594 1.002034 0.332638 0.027 Uiso 1 1 calc R . . . .
C33 C -0.0756(2) 1.08169(13) 0.33185(10) 0.0232(4) Uani 1 1 d . . . . .
H33 H -0.108037 1.131444 0.334268 0.028 Uiso 1 1 calc R . . . .
C34 C 0.0496(2) 1.08561(13) 0.32969(10) 0.0243(4) Uani 1 1 d . . . . .
H34 H 0.103772 1.138620 0.332098 0.029 Uiso 1 1 calc R . . . .
C35 C 0.0962(2) 1.01286(13) 0.32405(9) 0.0202(4) Uani 1 1 d . . . . .
H35 H 0.181429 1.015912 0.321438 0.024 Uiso 1 1 calc R . . . .
C36 C 0.09305(19) 0.42530(12) 0.23492(9) 0.0169(4) Uani 1 1 d . . . . .
C37 C 0.17014(19) 0.44442(12) 0.35005(9) 0.0161(4) Uani 1 1 d . . . . .
C38 C 0.29924(19) 0.45187(13) 0.37535(9) 0.0184(4) Uani 1 1 d . . . . .
C39 C 0.3292(2) 0.41862(15) 0.42739(10) 0.0257(5) Uani 1 1 d . . . . .
H39 H 0.415356 0.421998 0.445749 0.031 Uiso 1 1 calc R . . . .
C40 C 0.2360(2) 0.38075(15) 0.45292(11) 0.0276(5) Uani 1 1 d . . . . .
H40 H 0.258785 0.357209 0.487778 0.033 Uiso 1 1 calc R . . . .
C41 C 0.1105(2) 0.37685(14) 0.42826(10) 0.0237(4) Uani 1 1 d . . . . .
H41 H 0.047851 0.351746 0.446940 0.028 Uiso 1 1 calc R . . . .
C42 C 0.07402(19) 0.40932(12) 0.37613(9) 0.0182(4) Uani 1 1 d . . . . .
C43 C 0.40326(19) 0.49511(14) 0.34875(10) 0.0225(4) Uani 1 1 d . . . . .
H43 H 0.372225 0.540766 0.331159 0.027 Uiso 1 1 calc R . . . .
C44 C 0.5243(2) 0.53808(15) 0.39985(11) 0.0259(5) Uani 1 1 d . . . . .
H44A H 0.582518 0.574545 0.383035 0.039 Uiso 1 1 calc GR . . . .
H44B H 0.564484 0.494516 0.413559 0.039 Uiso 1 1 calc GR . . . .
H44C H 0.503282 0.572687 0.435704 0.039 Uiso 1 1 calc GR . . . .
C45 C 0.4348(2) 0.43497(17) 0.29520(11) 0.0328(5) Uani 1 1 d . . . . .
H45A H 0.457348 0.386179 0.309692 0.049 Uiso 1 1 calc GR . . . .
H45B H 0.506262 0.465391 0.282295 0.049 Uiso 1 1 calc GR . . . .
H45C H 0.361048 0.414921 0.259402 0.049 Uiso 1 1 calc GR . . . .
C46 C -0.06405(19) 0.40893(13) 0.35277(10) 0.0217(4) Uani 1 1 d . . . . .
H46 H -0.071156 0.437584 0.317232 0.026 Uiso 1 1 calc R . . . .
C47 C -0.1130(2) 0.45906(14) 0.40476(11) 0.0278(5) Uani 1 1 d . . . . .
H47A H -0.110473 0.430590 0.439353 0.042 Uiso 1 1 calc GR . . . .
H47B H -0.200278 0.461774 0.387847 0.042 Uiso 1 1 calc GR . . . .
H47C H -0.059536 0.516847 0.420309 0.042 Uiso 1 1 calc GR . . . .
C48 C -0.1462(2) 0.31807(15) 0.32824(12) 0.0324(5) Uani 1 1 d . . . . .
H48A H -0.233012 0.319980 0.309531 0.049 Uiso 1 1 calc GR . . . .
H48B H -0.146214 0.290290 0.363119 0.049 Uiso 1 1 calc GR . . . .
H48C H -0.111995 0.285869 0.296380 0.049 Uiso 1 1 calc GR . . . .
C49 C 0.0296(2) 0.45081(12) 0.12863(9) 0.0179(4) Uani 1 1 d . . . . .
C50 C 0.1061(2) 0.42212(13) 0.08993(9) 0.0216(4) Uani 1 1 d . . . . .
C51 C 0.0516(2) 0.39489(14) 0.02563(10) 0.0289(5) Uani 1 1 d . . . . .
H51 H 0.100828 0.375078 -0.002041 0.035 Uiso 1 1 calc R . . . .
C52 C -0.0720(2) 0.39601(15) 0.00124(11) 0.0329(5) Uani 1 1 d . . . . .
H52 H -0.107002 0.377088 -0.042772 0.039 Uiso 1 1 calc R . . . .
C53 C -0.1451(2) 0.42468(15) 0.04085(10) 0.0281(5) Uani 1 1 d . . . . .
H53 H -0.230319 0.424949 0.023522 0.034 Uiso 1 1 calc R . . . .
C54 C -0.0966(2) 0.45310(13) 0.10538(9) 0.0210(4) Uani 1 1 d . . . . .
C55 C 0.2424(2) 0.41861(15) 0.11408(10) 0.0272(5) Uani 1 1 d . . . . .
H55 H 0.268419 0.446662 0.160030 0.033 Uiso 1 1 calc R . . . .
C56 C 0.3307(2) 0.46711(16) 0.08138(12) 0.0328(5) Uani 1 1 d . . . . .
H56A H 0.318392 0.525140 0.085472 0.049 Uiso 1 1 calc GR . . . .
H56B H 0.311481 0.437953 0.036784 0.049 Uiso 1 1 calc GR . . . .
H56C H 0.418787 0.469217 0.101000 0.049 Uiso 1 1 calc GR . . . .
C57 C 0.2572(3) 0.32675(17) 0.10571(13) 0.0415(7) Uani 1 1 d . . . . .
H57A H 0.344712 0.326666 0.124699 0.062 Uiso 1 1 calc GR . . . .
H57B H 0.236631 0.298883 0.060810 0.062 Uiso 1 1 calc GR . . . .
H57C H 0.199847 0.295923 0.126255 0.062 Uiso 1 1 calc GR . . . .
C58 C -0.1808(2) 0.48475(14) 0.14702(10) 0.0240(4) Uani 1 1 d . . . . .
H58 H -0.132135 0.498688 0.191792 0.029 Uiso 1 1 calc R . . . .
C59 C -0.2157(2) 0.56534(16) 0.13309(12) 0.0328(5) Uani 1 1 d . . . . .
H59A H -0.266514 0.552553 0.089863 0.049 Uiso 1 1 calc GR . . . .
H59B H -0.138454 0.608618 0.138154 0.049 Uiso 1 1 calc GR . . . .
H59C H -0.264755 0.586714 0.162292 0.049 Uiso 1 1 calc GR . . . .
C60 C -0.3026(3) 0.41770(17) 0.13943(14) 0.0423(7) Uani 1 1 d . . . . .
H60A H -0.280911 0.366517 0.150164 0.063 Uiso 1 1 calc GR . . . .
H60B H -0.351983 0.403224 0.095817 0.063 Uiso 1 1 calc GR . . . .
H60C H -0.352741 0.440600 0.167476 0.063 Uiso 1 1 calc GR . . . .
C61 C 0.0590(2) 0.33137(13) 0.21641(10) 0.0233(4) Uani 1 1 d . . . . .
C62 C 0.1389(3) 0.28375(14) 0.24154(11) 0.0293(5) Uani 1 1 d . . . . .
H62 H 0.215356 0.311614 0.272014 0.035 Uiso 1 1 calc R . . . .
C63 C 0.1060(3) 0.19537(15) 0.22177(12) 0.0415(7) Uani 1 1 d . . . . .
H63 H 0.162025 0.163075 0.237397 0.050 Uiso 1 1 calc R . . . .
C64 C -0.0086(3) 0.15404(16) 0.17922(12) 0.0476(8) Uani 1 1 d . . . . .
H64 H -0.031495 0.093664 0.166614 0.057 Uiso 1 1 calc R . . . .
C65 C -0.0890(3) 0.20085(16) 0.15538(13) 0.0442(7) Uani 1 1 d . . . . .
H65 H -0.167808 0.172674 0.126886 0.053 Uiso 1 1 calc R . . . .
C66 C -0.0546(3) 0.28922(14) 0.17304(11) 0.0316(5) Uani 1 1 d . . . . .
H66 H -0.108926 0.321170 0.155403 0.038 Uiso 1 1 calc R . . . .
C67 C 0.43088(18) 0.72980(13) 0.47430(9) 0.0186(4) Uani 1 1 d . . . . .
C68 C 0.53583(19) 0.79650(14) 0.50503(10) 0.0238(4) Uani 1 1 d . . . . .
H68 H 0.574503 0.831199 0.481559 0.029 Uiso 1 1 calc R . . . .
C69 C 0.5844(2) 0.81273(16) 0.56956(11) 0.0307(5) Uani 1 1 d . . . . .
H69 H 0.656290 0.858029 0.589579 0.037 Uiso 1 1 calc R . . . .
C70 C 0.5293(2) 0.76372(17) 0.60471(11) 0.0324(5) Uani 1 1 d . . . . .
H70 H 0.561417 0.775791 0.648897 0.039 Uiso 1 1 calc R . . . .
C71 C 0.4260(2) 0.69647(15) 0.57464(10) 0.0265(5) Uani 1 1 d . . . . .
H71 H 0.387364 0.662348 0.598468 0.032 Uiso 1 1 calc R . . . .
C72 C 0.37887(19) 0.67868(14) 0.51018(10) 0.0211(4) Uani 1 1 d . . . . .
H72 H 0.310305 0.631110 0.490107 0.025 Uiso 1 1 calc R . . . .
C73 C 0.3825(2) 0.70945(14) 0.13227(10) 0.0257(5) Uani 1 1 d . . . . .
C74 C 0.4782(2) 0.68526(18) 0.10469(12) 0.0365(6) Uani 1 1 d . . . . .
H74 H 0.525059 0.648430 0.121035 0.044 Uiso 1 1 calc R . . . .
C75 C 0.5046(3) 0.7149(2) 0.05363(13) 0.0480(8) Uani 1 1 d . . . . .
H75 H 0.569128 0.697759 0.035147 0.058 Uiso 1 1 calc R . . . .
C76 C 0.4385(3) 0.7690(2) 0.02935(13) 0.0509(8) Uani 1 1 d . . . . .
H76 H 0.456903 0.788692 -0.005758 0.061 Uiso 1 1 calc R . . . .
C77 C 0.3447(3) 0.79423(17) 0.05684(13) 0.0429(7) Uani 1 1 d . . . . .
H77 H 0.299121 0.831797 0.040675 0.051 Uiso 1 1 calc R . . . .
C78 C 0.3174(2) 0.76474(15) 0.10785(11) 0.0308(5) Uani 1 1 d . . . . .
H78 H 0.253383 0.782595 0.126359 0.037 Uiso 1 1 calc R . . . .
C79 C 0.6240(3) 0.1355(2) 0.21318(18) 0.0585(9) Uani 1 1 d . . . . .
H79 H 0.664028 0.154537 0.256687 0.070 Uiso 1 1 calc R . . . .
C80 C 0.6387(3) 0.0601(2) 0.17820(17) 0.0522(8) Uani 1 1 d . . . . .
H80 H 0.690142 0.028170 0.197940 0.063 Uiso 1 1 calc R . . . .
C81 C 0.5806(3) 0.0310(2) 0.11593(16) 0.0527(8) Uani 1 1 d . . . . .
H81 H 0.590437 -0.021046 0.092388 0.063 Uiso 1 1 calc R . . . .
C82 C 0.5070(4) 0.0786(3) 0.08760(18) 0.0653(10) Uani 1 1 d . . . . .
H82 H 0.465999 0.058953 0.044238 0.078 Uiso 1 1 calc R . . . .
C83 C 0.4927(4) 0.1541(2) 0.12156(19) 0.0662(10) Uani 1 1 d . . . . .
H83 H 0.442668 0.186655 0.101615 0.079 Uiso 1 1 calc R . . . .
C84 C 0.5513(4) 0.1824(2) 0.18468(19) 0.0649(10) Uani 1 1 d . . . . .
H84 H 0.541240 0.234312 0.208369 0.078 Uiso 1 1 calc R . . . .
C85 C 0.1154(3) 0.0571(2) 0.01361(13) 0.0503(8) Uani 1 1 d . . . . .
H85 H 0.194999 0.096279 0.023020 0.060 Uiso 1 1 calc R . . . .
C86 C 0.0112(3) 0.0851(2) 0.02656(13) 0.0499(8) Uani 1 1 d . . . . .
H86 H 0.018914 0.143543 0.044721 0.060 Uiso 1 1 calc R . . . .
C87 C -0.1040(3) 0.0284(2) 0.01323(13) 0.0503(8) Uani 1 1 d . . . . .
H87 H -0.175695 0.047707 0.022366 0.060 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'
Ge Ge 0.1547 1.8001 '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'
S S 0.1246 0.1234 '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 -5 3 0.0338
-1 5 -3 0.0338
1 -14 -20 0.0712
16 -5 -8 0.1673
0 14 19 0.0608
5 -1 -2 0.1664
0 3 5 0.0706
-5 -3 -4 0.1296
0 -4 5 0.0804
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 Ge1 S1 91.38(5) . . ?
C3 Ge1 S1 97.08(5) . . ?
C3 Ge1 C1 89.62(7) . . ?
C2 Ge2 S2 101.81(5) . . ?
C2 Ge2 C4 91.05(7) . . ?
C4 Ge2 S2 92.55(5) . . ?
C67 S1 Ge1 103.95(7) . . ?
C73 S2 Ge2 102.79(8) . . ?
C1 N1 C6 124.52(15) . . ?
C5 N1 C1 110.38(15) . . ?
C5 N1 C6 124.29(15) . . ?
C2 N2 C18 126.28(15) . . ?
C5 N2 C2 110.86(15) . . ?
C5 N2 C18 122.44(16) . . ?
C3 N3 C37 124.18(15) . . ?
C36 N3 C3 110.58(15) . . ?
C36 N3 C37 125.18(16) . . ?
C4 N4 C49 124.75(16) . . ?
C36 N4 C4 110.19(15) . . ?
C36 N4 C49 124.91(16) . . ?
N1 C1 Ge1 120.76(13) . . ?
C2 C1 Ge1 130.56(14) . . ?
C2 C1 N1 106.22(16) . . ?
N2 C2 Ge2 120.28(13) . . ?
C1 C2 Ge2 128.60(14) . . ?
C1 C2 N2 105.97(15) . . ?
N3 C3 Ge1 119.40(13) . . ?
C4 C3 Ge1 131.77(14) . . ?
C4 C3 N3 106.14(16) . . ?
N4 C4 Ge2 121.23(13) . . ?
C3 C4 Ge2 132.05(14) . . ?
C3 C4 N4 106.31(16) . . ?
N1 C5 N2 106.45(16) . . ?
N1 C5 C30 127.72(17) . . ?
N2 C5 C30 125.69(17) . . ?
C7 C6 N1 119.25(17) . . ?
C7 C6 C11 123.63(17) . . ?
C11 C6 N1 117.11(16) . . ?
C6 C7 C12 123.32(17) . . ?
C8 C7 C6 116.70(18) . . ?
C8 C7 C12 119.98(18) . . ?
C9 C8 C7 121.27(19) . . ?
C8 C9 C10 120.65(19) . . ?
C9 C10 C11 120.97(19) . . ?
C6 C11 C15 122.39(17) . . ?
C10 C11 C6 116.73(18) . . ?
C10 C11 C15 120.86(17) . . ?
C7 C12 C13 111.24(18) . . ?
C7 C12 C14 111.08(19) . . ?
C14 C12 C13 110.23(18) . . ?
C11 C15 C16 113.25(17) . . ?
C11 C15 C17 110.07(16) . . ?
C17 C15 C16 109.97(17) . . ?
C19 C18 N2 119.31(16) . . ?
C19 C18 C23 123.71(18) . . ?
C23 C18 N2 116.85(17) . . ?
C18 C19 C24 123.13(17) . . ?
C20 C19 C18 116.92(18) . . ?
C20 C19 C24 119.92(18) . . ?
C21 C20 C19 121.0(2) . . ?
C20 C21 C22 120.7(2) . . ?
C21 C22 C23 121.1(2) . . ?
C18 C23 C27 122.30(18) . . ?
C22 C23 C18 116.4(2) . . ?
C22 C23 C27 121.28(18) . . ?
C19 C24 C25 112.46(17) . . ?
C19 C24 C26 109.78(16) . . ?
C26 C24 C25 110.30(17) . . ?
C23 C27 C28 112.71(18) . . ?
C23 C27 C29 112.22(19) . . ?
C29 C27 C28 109.56(19) . . ?
C31 C30 C5 119.90(17) . . ?
C31 C30 C35 118.88(18) . . ?
C35 C30 C5 121.15(17) . . ?
C32 C31 C30 120.49(19) . . ?
C33 C32 C31 120.17(19) . . ?
C32 C33 C34 119.62(19) . . ?
C35 C34 C33 120.42(19) . . ?
C34 C35 C30 120.39(19) . . ?
N3 C36 N4 106.68(16) . . ?
N3 C36 C61 126.74(18) . . ?
N4 C36 C61 126.52(18) . . ?
C38 C37 N3 117.63(17) . . ?
C42 C37 N3 119.01(17) . . ?
C42 C37 C38 123.36(18) . . ?
C37 C38 C43 122.72(17) . . ?
C39 C38 C37 116.66(18) . . ?
C39 C38 C43 120.61(19) . . ?
C40 C39 C38 121.3(2) . . ?
C41 C40 C39 120.6(2) . . ?
C40 C41 C42 120.94(19) . . ?
C37 C42 C46 123.44(18) . . ?
C41 C42 C37 117.02(19) . . ?
C41 C42 C46 119.47(18) . . ?
C38 C43 C44 111.78(17) . . ?
C38 C43 C45 113.47(19) . . ?
C44 C43 C45 109.32(18) . . ?
C42 C46 C47 110.74(17) . . ?
C42 C46 C48 111.60(18) . . ?
C48 C46 C47 110.13(18) . . ?
C50 C49 N4 118.88(18) . . ?
C50 C49 C54 123.00(18) . . ?
C54 C49 N4 118.11(17) . . ?
C49 C50 C55 123.86(18) . . ?
C51 C50 C49 117.0(2) . . ?
C51 C50 C55 119.18(19) . . ?
C52 C51 C50 121.6(2) . . ?
C51 C52 C53 120.0(2) . . ?
C52 C53 C54 121.5(2) . . ?
C49 C54 C58 123.53(18) . . ?
C53 C54 C49 117.0(2) . . ?
C53 C54 C58 119.5(2) . . ?
C50 C55 C56 111.16(19) . . ?
C50 C55 C57 111.5(2) . . ?
C57 C55 C56 109.87(19) . . ?
C54 C58 C60 112.52(19) . . ?
C59 C58 C54 110.88(18) . . ?
C59 C58 C60 109.0(2) . . ?
C62 C61 C36 121.1(2) . . ?
C66 C61 C36 119.6(2) . . ?
C66 C61 C62 119.2(2) . . ?
C63 C62 C61 119.8(3) . . ?
C62 C63 C64 120.4(3) . . ?
C65 C64 C63 119.9(2) . . ?
C64 C65 C66 120.0(3) . . ?
C65 C66 C61 120.6(3) . . ?
C68 C67 S1 117.67(16) . . ?
C68 C67 C72 117.84(19) . . ?
C72 C67 S1 124.49(15) . . ?
C69 C68 C67 120.9(2) . . ?
C70 C69 C68 120.6(2) . . ?
C69 C70 C71 119.1(2) . . ?
C72 C71 C70 120.6(2) . . ?
C71 C72 C67 120.9(2) . . ?
C74 C73 S2 118.2(2) . . ?
C78 C73 S2 123.54(17) . . ?
C78 C73 C74 118.3(2) . . ?
C75 C74 C73 120.3(3) . . ?
C76 C75 C74 120.9(3) . . ?
C75 C76 C77 119.3(3) . . ?
C78 C77 C76 120.2(3) . . ?
C77 C78 C73 121.0(2) . . ?
C84 C79 C80 119.6(4) . . ?
C81 C80 C79 121.1(3) . . ?
C80 C81 C82 118.9(3) . . ?
C83 C82 C81 120.7(4) . . ?
C82 C83 C84 119.7(4) . . ?
C79 C84 C83 119.9(3) . . ?
C86 C85 C87 119.9(3) . 2 ?
C87 C86 C85 120.1(3) . . ?
C86 C87 C85 119.9(3) . 2 ?
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
Ge1 S1 2.3604(5) . ?
Ge1 C1 2.0286(19) . ?
Ge1 C3 2.0250(18) . ?
Ge2 S2 2.3389(5) . ?
Ge2 C2 2.0279(18) . ?
Ge2 C4 2.0333(19) . ?
S1 C67 1.769(2) . ?
S2 C73 1.775(2) . ?
N1 C1 1.409(2) . ?
N1 C5 1.347(2) . ?
N1 C6 1.444(2) . ?
N2 C2 1.402(2) . ?
N2 C5 1.348(2) . ?
N2 C18 1.442(2) . ?
N3 C3 1.405(2) . ?
N3 C36 1.348(2) . ?
N3 C37 1.453(2) . ?
N4 C4 1.411(2) . ?
N4 C36 1.348(2) . ?
N4 C49 1.455(2) . ?
C1 C2 1.378(3) . ?
C3 C4 1.375(3) . ?
C5 C30 1.476(3) . ?
C6 C7 1.396(3) . ?
C6 C11 1.406(3) . ?
C7 C8 1.395(3) . ?
C7 C12 1.514(3) . ?
C8 C9 1.378(3) . ?
C9 C10 1.384(3) . ?
C10 C11 1.394(3) . ?
C11 C15 1.515(3) . ?
C12 C13 1.534(3) . ?
C12 C14 1.532(3) . ?
C15 C16 1.536(3) . ?
C15 C17 1.529(3) . ?
C18 C19 1.394(3) . ?
C18 C23 1.408(3) . ?
C19 C20 1.394(3) . ?
C19 C24 1.517(3) . ?
C20 C21 1.379(3) . ?
C21 C22 1.384(3) . ?
C22 C23 1.393(3) . ?
C23 C27 1.523(3) . ?
C24 C25 1.532(3) . ?
C24 C26 1.532(3) . ?
C27 C28 1.530(3) . ?
C27 C29 1.525(3) . ?
C30 C31 1.391(3) . ?
C30 C35 1.398(3) . ?
C31 C32 1.391(3) . ?
C32 C33 1.385(3) . ?
C33 C34 1.387(3) . ?
C34 C35 1.382(3) . ?
C36 C61 1.477(3) . ?
C37 C38 1.405(3) . ?
C37 C42 1.398(3) . ?
C38 C39 1.391(3) . ?
C38 C43 1.523(3) . ?
C39 C40 1.383(3) . ?
C40 C41 1.377(3) . ?
C41 C42 1.398(3) . ?
C42 C46 1.516(3) . ?
C43 C44 1.530(3) . ?
C43 C45 1.535(3) . ?
C46 C47 1.534(3) . ?
C46 C48 1.534(3) . ?
C49 C50 1.399(3) . ?
C49 C54 1.404(3) . ?
C50 C51 1.393(3) . ?
C50 C55 1.518(3) . ?
C51 C52 1.376(4) . ?
C52 C53 1.383(3) . ?
C53 C54 1.389(3) . ?
C54 C58 1.526(3) . ?
C55 C56 1.534(3) . ?
C55 C57 1.531(3) . ?
C58 C59 1.523(3) . ?
C58 C60 1.536(3) . ?
C61 C62 1.397(3) . ?
C61 C66 1.395(3) . ?
C62 C63 1.392(3) . ?
C63 C64 1.392(4) . ?
C64 C65 1.380(4) . ?
C65 C66 1.390(3) . ?
C67 C68 1.397(3) . ?
C67 C72 1.398(3) . ?
C68 C69 1.392(3) . ?
C69 C70 1.379(4) . ?
C70 C71 1.389(3) . ?
C71 C72 1.386(3) . ?
C73 C74 1.404(3) . ?
C73 C78 1.391(3) . ?
C74 C75 1.388(4) . ?
C75 C76 1.379(5) . ?
C76 C77 1.391(4) . ?
C77 C78 1.389(3) . ?
C79 C80 1.385(5) . ?
C79 C84 1.371(5) . ?
C80 C81 1.363(5) . ?
C81 C82 1.383(5) . ?
C82 C83 1.376(5) . ?
C83 C84 1.380(5) . ?
C85 C86 1.378(5) . ?
C85 C87 1.390(4) 2 ?
C86 C87 1.376(4) . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0.9947 -5.0088 2.9929 -0.1970 -0.0567 -0.0934
-0.9947 5.0088 -2.9929 0.1970 0.0567 0.0934
0.7966 -13.8528 -19.8457 -0.0683 0.3766 -0.9238
15.5766 -4.5236 -7.9273 0.1613 -0.8613 -0.4819
0.3549 13.5922 19.3651 0.0806 -0.4426 0.8931
4.9998 -1.0006 -1.9997 0.0561 -0.2890 -0.1273
0.0045 2.9937 4.9994 0.0040 -0.1032 0.2153
-5.0057 -2.9921 -4.0000 -0.0732 0.4170 -0.1436
-0.0039 -4.0108 4.9925 -0.2118 -0.0303 -0.0041
