#------------------------------------------------------------------------------
#$Date: 2020-12-31 01:58:24 +0200 (Thu, 31 Dec 2020) $
#$Revision: 260256 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/54/4135439.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_4135439
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         'C66 H78 Cl2 Ge2 N4, 2(C4 H8 O)'
_chemical_formula_sum            'C74 H94 Cl2 Ge2 N4 O2'
_chemical_formula_weight         1287.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-13
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.358(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7437(4)
_cell_length_b                   20.2913(4)
_cell_length_c                   24.8641(4)
_cell_measurement_reflns_used    40383
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      29.5630
_cell_measurement_theta_min      1.5060
_cell_volume                     6860.4(3)
_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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     17.00  94.00   1.00   45.00    --   24.79-148.00 -20.41   77
  2  ω     -4.00  42.00   1.00   45.00    --   24.79  77.00-120.00   46
  3  ω      3.00  95.00   1.00   45.00    --   24.79  38.00  30.00   92
  4  ω      6.00  93.00   1.00   45.00    --   24.79  57.00 -90.00   87
  5  ω     39.00  99.00   1.00   45.00    --   24.79 178.00-120.00   60
  6  ω    -44.00  43.00   1.00   45.00    --   24.79 -57.00 -30.00   87
  7  ω    -44.00  43.00   1.00   45.00    --   24.79 -57.00-150.00   87
  8  ω     -4.00  42.00   1.00   45.00    --   24.79  77.00   0.00   46
  9  ω    -46.00  96.00   1.00   45.00    --   24.79   0.00 -30.00  142
 10  ω    -46.00  47.00   1.00   45.00    --   24.79 -38.00-120.00   93
 11  ω      6.00  93.00   1.00   45.00    --   24.79  57.00 150.00   87
 12  ω      7.00  80.00   1.00   45.00    --   24.79-126.00-173.03   73
 13  ω      6.00  93.00   1.00   45.00    --   24.79  57.00  60.00   87
 14  ω      2.00  77.00   1.00   45.00    --   24.79-120.00  95.72   75
 15  ω    -95.00  48.00   1.00   45.00    --  -23.50   0.00-150.00  143
 16  ω    -95.00  48.00   1.00   45.00    --  -23.50   0.00-180.00  143
 17  ω    -95.00  48.00   1.00   45.00    --  -23.50   0.00-120.00  143
 18  ω    -97.00 -39.00   1.00   45.00    --  -23.50-178.00 -30.00   58
 19  ω    -15.00  65.00   1.00   45.00    --   24.79 -99.00   0.00   80
 20  ω     -4.00  42.00   1.00   45.00    --   24.79  77.00-180.00   46
 21  ω     -4.00   7.00   1.00   45.00    --   24.79  77.00 -90.00   11
;
_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      0.0497404000
_diffrn_orient_matrix_UB_12      0.0067803000
_diffrn_orient_matrix_UB_13      0.0105913000
_diffrn_orient_matrix_UB_21      0.0104125000
_diffrn_orient_matrix_UB_22      -0.0342458000
_diffrn_orient_matrix_UB_23      0.0006981000
_diffrn_orient_matrix_UB_31      0.0117673000
_diffrn_orient_matrix_UB_32      0.0017788000
_diffrn_orient_matrix_UB_33      -0.0268085000
_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  0.0987
_diffrn_reflns_av_unetI/netI     0.0738
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            172538
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.498
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.394
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         13326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0515
_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)+(0.0713P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1263
_refine_ls_wR_factor_ref         0.1325
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8674
_reflns_number_total             13326
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by -175.9596° 
 around [-0.00 1.00 0.01] (reciprocal) or [-0.01 1.00 0.01] (direct)
;
_cod_data_source_file            ja0c11828_si_002.cif
_cod_data_source_block           compound2
_cod_database_code               4135439
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C74H94Cl2Ge2N4O2
_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   0.840
_shelx_estimated_absorpt_t_min   0.751
_diffrn_oxdiff_digest_frames
;
0121d3967fc7e636a1b558622b753c2f8901765393e
;
_diffrn_oxdiff_digest_hkl
;
012606e48db69e3d6f69d80c90a665fc9a1cf9
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C72B) = Uanis(C72)
Uanis(C73) = Uanis(C73B)
Uanis(O2B) = Uanis(O2)
3. Others
 Sof(O2B)=Sof(H71C)=Sof(H71D)=Sof(C72B)=Sof(H72C)=Sof(H72D)=Sof(C73B)=
 Sof(H73C)=Sof(H73D)=Sof(H74C)=Sof(H74D)=1-FVAR(1)
 Sof(O2)=Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)=Sof(H73A)=
 Sof(H73B)=Sof(H74A)=Sof(H74B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19), C28(H28), C31(H31), C49(H49), C52(H52), C61(H61), C64(H64)
4.b Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C71(H71C,
 H71D), C71(H71A,H71B), C72(H72A,H72B), C72B(H72C,H72D), C73(H73A,H73B),
 C73B(H73C,H73D), C74(H74A,H74B), C74(H74C,H74D)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C24(H24), C25(H25), C26(H26), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C45(H45), C46(H46), C47(H47), C57(H57), C58(H58), C59(H59)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C)
;
_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 2.176
_oxdiff_exptl_absorpt_empirical_full_min 0.591
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_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 0.80975(3) 0.55354(2) 0.81050(2) 0.01908(11) Uani 1 1 d . . . . .
Ge2 Ge 0.68375(3) 0.44767(2) 0.67554(2) 0.01975(11) Uani 1 1 d . . . . .
Cl1 Cl 0.69960(8) 0.64100(5) 0.79272(4) 0.0373(3) Uani 1 1 d . . . . .
Cl2 Cl 0.79813(8) 0.36908(5) 0.71366(4) 0.0428(3) Uani 1 1 d . . . . .
N1 N 0.9119(2) 0.58633(13) 0.71622(10) 0.0165(6) Uani 1 1 d . . . . .
N2 N 0.8364(2) 0.54121(13) 0.64300(10) 0.0169(6) Uani 1 1 d . . . . .
N3 N 0.6466(2) 0.46982(13) 0.83966(10) 0.0159(6) Uani 1 1 d . . . . .
N4 N 0.5628(2) 0.43199(13) 0.76587(10) 0.0155(6) Uani 1 1 d . . . . .
C1 C 0.8330(2) 0.55017(16) 0.73188(12) 0.0165(7) Uani 1 1 d . . . . .
C2 C 0.7861(2) 0.52067(17) 0.68614(12) 0.0168(7) Uani 1 1 d . . . . .
C3 C 0.9109(2) 0.58082(16) 0.66194(12) 0.0170(7) Uani 1 1 d . . . . .
C4 C 0.9783(2) 0.61559(17) 0.62978(12) 0.0184(7) Uani 1 1 d . . . . .
C5 C 1.0786(3) 0.62216(17) 0.64834(13) 0.0222(8) Uani 1 1 d . . . . .
H5 H 1.106291 0.601916 0.681503 0.027 Uiso 1 1 calc R . . . .
C6 C 1.1381(3) 0.65819(17) 0.61852(14) 0.0254(8) Uani 1 1 d . . . . .
H6 H 1.206352 0.662535 0.631451 0.031 Uiso 1 1 calc R . . . .
C7 C 1.0986(3) 0.68779(18) 0.57010(13) 0.0269(9) Uani 1 1 d . . . . .
H7 H 1.139526 0.712540 0.549893 0.032 Uiso 1 1 calc R . . . .
C8 C 0.9995(3) 0.68118(17) 0.55129(13) 0.0249(8) Uani 1 1 d . . . . .
H8 H 0.972174 0.701154 0.517940 0.030 Uiso 1 1 calc R . . . .
C9 C 0.9402(3) 0.64555(17) 0.58092(13) 0.0225(8) Uani 1 1 d . . . . .
H9 H 0.872063 0.641423 0.567700 0.027 Uiso 1 1 calc R . . . .
C10 C 0.9870(3) 0.62086(17) 0.75298(12) 0.0187(8) Uani 1 1 d . . . . .
C11 C 0.9869(3) 0.68968(17) 0.75375(12) 0.0209(8) Uani 1 1 d . . . . .
C12 C 1.0656(3) 0.72061(19) 0.78519(13) 0.0302(9) Uani 1 1 d . . . . .
H12 H 1.068251 0.767381 0.786246 0.036 Uiso 1 1 calc R . . . .
C13 C 1.1396(3) 0.68484(19) 0.81480(14) 0.0319(10) Uani 1 1 d . . . . .
H13 H 1.193516 0.706938 0.835378 0.038 Uiso 1 1 calc R . . . .
C14 C 1.1357(3) 0.61598(19) 0.81475(14) 0.0304(9) Uani 1 1 d . . . . .
H14 H 1.186506 0.591758 0.836102 0.036 Uiso 1 1 calc R . . . .
C15 C 1.0590(3) 0.58251(18) 0.78403(13) 0.0225(8) Uani 1 1 d . . . . .
C16 C 0.9065(3) 0.73159(17) 0.72190(13) 0.0249(8) Uani 1 1 d . . . . .
H16 H 0.856715 0.701439 0.701417 0.030 Uiso 1 1 calc R . . . .
C17 C 0.9482(3) 0.77600(18) 0.68080(13) 0.0329(10) Uani 1 1 d . . . . .
H17A H 0.894059 0.798058 0.657678 0.049 Uiso 1 1 calc GR . . . .
H17B H 0.985532 0.749149 0.658172 0.049 Uiso 1 1 calc GR . . . .
H17C H 0.991684 0.809141 0.700312 0.049 Uiso 1 1 calc GR . . . .
C18 C 0.8546(3) 0.77377(18) 0.76058(14) 0.0337(10) Uani 1 1 d . . . . .
H18A H 0.829643 0.745176 0.787242 0.051 Uiso 1 1 calc GR . . . .
H18B H 0.799732 0.797616 0.739633 0.051 Uiso 1 1 calc GR . . . .
H18C H 0.901489 0.805413 0.779516 0.051 Uiso 1 1 calc GR . . . .
C19 C 1.0568(3) 0.50739(18) 0.78433(14) 0.0282(9) Uani 1 1 d . . . . .
H19 H 0.988801 0.493279 0.768781 0.034 Uiso 1 1 calc R . . . .
C20 C 1.0783(4) 0.4802(2) 0.84193(16) 0.0488(12) Uani 1 1 d . . . . .
H20A H 1.147299 0.488573 0.856629 0.073 Uiso 1 1 calc GR . . . .
H20B H 1.065795 0.432687 0.841378 0.073 Uiso 1 1 calc GR . . . .
H20C H 1.035672 0.502010 0.864855 0.073 Uiso 1 1 calc GR . . . .
C21 C 1.1273(3) 0.4777(2) 0.74925(16) 0.0444(11) Uani 1 1 d . . . . .
H21A H 1.111981 0.494712 0.712103 0.067 Uiso 1 1 calc GR . . . .
H21B H 1.120492 0.429604 0.748811 0.067 Uiso 1 1 calc GR . . . .
H21C H 1.194963 0.489573 0.764219 0.067 Uiso 1 1 calc GR . . . .
C22 C 0.8130(3) 0.51909(17) 0.58710(12) 0.0182(8) Uani 1 1 d . . . . .
C23 C 0.8689(3) 0.46772(17) 0.56979(12) 0.0214(8) Uani 1 1 d . . . . .
C24 C 0.8477(3) 0.44964(19) 0.51528(13) 0.0304(9) Uani 1 1 d . . . . .
H24 H 0.885327 0.415877 0.501647 0.036 Uiso 1 1 calc R . . . .
C25 C 0.7735(3) 0.4796(2) 0.48081(14) 0.0340(10) Uani 1 1 d . . . . .
H25 H 0.760189 0.466124 0.443888 0.041 Uiso 1 1 calc R . . . .
C26 C 0.7181(3) 0.5294(2) 0.49955(13) 0.0303(9) Uani 1 1 d . . . . .
H26 H 0.666504 0.549351 0.475421 0.036 Uiso 1 1 calc R . . . .
C27 C 0.7370(3) 0.55045(19) 0.55293(13) 0.0265(8) Uani 1 1 d . . . . .
C28 C 0.9489(3) 0.43133(18) 0.60611(13) 0.0264(9) Uani 1 1 d . . . . .
H28 H 0.947155 0.445975 0.644364 0.032 Uiso 1 1 calc R . . . .
C29 C 1.0506(3) 0.4475(2) 0.59176(15) 0.0349(9) Uani 1 1 d . . . . .
H29A H 1.059917 0.495431 0.592170 0.052 Uiso 1 1 calc GR . . . .
H29B H 1.056015 0.430447 0.555446 0.052 Uiso 1 1 calc GR . . . .
H29C H 1.101161 0.427136 0.618452 0.052 Uiso 1 1 calc GR . . . .
C30 C 0.9300(3) 0.35682(18) 0.60341(14) 0.0347(10) Uani 1 1 d . . . . .
H30A H 0.863397 0.347755 0.611133 0.052 Uiso 1 1 calc GR . . . .
H30B H 0.977947 0.334489 0.630384 0.052 Uiso 1 1 calc GR . . . .
H30C H 0.936684 0.340614 0.566999 0.052 Uiso 1 1 calc GR . . . .
C31 C 0.6786(3) 0.6088(2) 0.57232(15) 0.0428(12) Uani 1 1 d . . . . .
H31 H 0.714506 0.625183 0.607674 0.051 Uiso 1 1 calc R . . . .
C32 C 0.6651(3) 0.6662(2) 0.53254(18) 0.0519(12) Uani 1 1 d . . . . .
H32A H 0.729076 0.678943 0.522825 0.078 Uiso 1 1 calc GR . . . .
H32B H 0.636305 0.703654 0.549458 0.078 Uiso 1 1 calc GR . . . .
H32C H 0.621196 0.652865 0.499701 0.078 Uiso 1 1 calc GR . . . .
C33 C 0.5785(4) 0.5841(3) 0.5818(2) 0.0785(19) Uani 1 1 d . . . . .
H33A H 0.541365 0.569360 0.547237 0.118 Uiso 1 1 calc GR . . . .
H33B H 0.542586 0.619787 0.596819 0.118 Uiso 1 1 calc GR . . . .
H33C H 0.586663 0.547178 0.607456 0.118 Uiso 1 1 calc GR . . . .
C34 C 0.6968(2) 0.48911(15) 0.79663(12) 0.0147(7) Uani 1 1 d . . . . .
C35 C 0.6447(2) 0.46391(16) 0.75017(12) 0.0159(7) Uani 1 1 d . . . . .
C36 C 0.5658(2) 0.43553(16) 0.82031(12) 0.0158(7) Uani 1 1 d . . . . .
C37 C 0.4942(2) 0.40504(16) 0.85201(12) 0.0183(8) Uani 1 1 d . . . . .
C38 C 0.5261(3) 0.37205(17) 0.90094(12) 0.0230(8) Uani 1 1 d . . . . .
H38 H 0.594233 0.370291 0.914675 0.028 Uiso 1 1 calc R . . . .
C39 C 0.4588(3) 0.34201(18) 0.92934(13) 0.0270(9) Uani 1 1 d . . . . .
H39 H 0.481087 0.319502 0.962337 0.032 Uiso 1 1 calc R . . . .
C40 C 0.3599(3) 0.34451(19) 0.91016(14) 0.0305(9) Uani 1 1 d . . . . .
H40 H 0.313981 0.324289 0.930097 0.037 Uiso 1 1 calc R . . . .
C41 C 0.3274(3) 0.37638(19) 0.86201(14) 0.0274(9) Uani 1 1 d . . . . .
H41 H 0.259148 0.377368 0.848440 0.033 Uiso 1 1 calc R . . . .
C42 C 0.3938(3) 0.40706(17) 0.83319(13) 0.0235(8) Uani 1 1 d . . . . .
H42 H 0.370596 0.429627 0.800347 0.028 Uiso 1 1 calc R . . . .
C43 C 0.6829(2) 0.48040(16) 0.89686(12) 0.0165(7) Uani 1 1 d . . . . .
C44 C 0.6341(2) 0.52628(17) 0.92582(12) 0.0192(8) Uani 1 1 d . . . . .
C45 C 0.6629(3) 0.52865(18) 0.98198(13) 0.0251(9) Uani 1 1 d . . . . .
H45 H 0.629752 0.557644 1.003217 0.030 Uiso 1 1 calc R . . . .
C46 C 0.7379(3) 0.49019(18) 1.00721(13) 0.0270(9) Uani 1 1 d . . . . .
H46 H 0.755242 0.492478 1.045570 0.032 Uiso 1 1 calc R . . . .
C47 C 0.7891(3) 0.44764(18) 0.97717(13) 0.0248(8) Uani 1 1 d . . . . .
H47 H 0.842258 0.422377 0.995175 0.030 Uiso 1 1 calc R . . . .
C48 C 0.7630(3) 0.44183(17) 0.92101(12) 0.0197(8) Uani 1 1 d . . . . .
C49 C 0.5561(3) 0.57322(18) 0.89940(13) 0.0221(8) Uani 1 1 d . . . . .
H49 H 0.550374 0.567301 0.859131 0.027 Uiso 1 1 calc R . . . .
C50 C 0.5861(3) 0.64511(18) 0.91261(14) 0.0292(9) Uani 1 1 d . . . . .
H50A H 0.589502 0.652678 0.951769 0.044 Uiso 1 1 calc GR . . . .
H50B H 0.537312 0.674826 0.892792 0.044 Uiso 1 1 calc GR . . . .
H50C H 0.650670 0.653624 0.901702 0.044 Uiso 1 1 calc GR . . . .
C51 C 0.4552(3) 0.5594(2) 0.91614(15) 0.0342(9) Uani 1 1 d . . . . .
H51A H 0.436768 0.513457 0.907819 0.051 Uiso 1 1 calc GR . . . .
H51B H 0.406151 0.588756 0.896081 0.051 Uiso 1 1 calc GR . . . .
H51C H 0.458048 0.567105 0.955250 0.051 Uiso 1 1 calc GR . . . .
C52 C 0.8201(3) 0.39630(17) 0.88792(13) 0.0232(8) Uani 1 1 d . . . . .
H52 H 0.830406 0.420912 0.854352 0.028 Uiso 1 1 calc R . . . .
C53 C 0.9211(3) 0.3788(2) 0.91762(14) 0.0323(9) Uani 1 1 d . . . . .
H53A H 0.957025 0.419313 0.929181 0.048 Uiso 1 1 calc GR . . . .
H53B H 0.957488 0.353873 0.893296 0.048 Uiso 1 1 calc GR . . . .
H53C H 0.913994 0.351982 0.949588 0.048 Uiso 1 1 calc GR . . . .
C54 C 0.7643(3) 0.33329(19) 0.86948(15) 0.0352(10) Uani 1 1 d . . . . .
H54A H 0.753071 0.307611 0.901391 0.053 Uiso 1 1 calc GR . . . .
H54B H 0.802968 0.307116 0.847109 0.053 Uiso 1 1 calc GR . . . .
H54C H 0.700888 0.344718 0.848094 0.053 Uiso 1 1 calc GR . . . .
C55 C 0.4837(3) 0.40390(17) 0.72786(12) 0.0192(8) Uani 1 1 d . . . . .
C56 C 0.4740(3) 0.33528(17) 0.72412(12) 0.0225(8) Uani 1 1 d . . . . .
C57 C 0.3941(3) 0.31092(19) 0.68854(13) 0.0293(9) Uani 1 1 d . . . . .
H57 H 0.384633 0.264638 0.685246 0.035 Uiso 1 1 calc R . . . .
C58 C 0.3286(3) 0.3528(2) 0.65804(14) 0.0346(10) Uani 1 1 d . . . . .
H58 H 0.274555 0.335165 0.634208 0.042 Uiso 1 1 calc R . . . .
C59 C 0.3417(3) 0.42025(19) 0.66217(14) 0.0287(9) Uani 1 1 d . . . . .
H59 H 0.296102 0.448443 0.640931 0.034 Uiso 1 1 calc R . . . .
C60 C 0.4195(3) 0.44783(18) 0.69647(13) 0.0234(8) Uani 1 1 d . . . . .
C61 C 0.5457(3) 0.28839(17) 0.75624(13) 0.0272(9) Uani 1 1 d . . . . .
H61 H 0.597366 0.315456 0.778572 0.033 Uiso 1 1 calc R . . . .
C62 C 0.5971(3) 0.24500(19) 0.71805(16) 0.0401(11) Uani 1 1 d . . . . .
H62A H 0.548602 0.216193 0.696939 0.060 Uiso 1 1 calc GR . . . .
H62B H 0.647641 0.218065 0.739635 0.060 Uiso 1 1 calc GR . . . .
H62C H 0.627914 0.273148 0.693267 0.060 Uiso 1 1 calc GR . . . .
C63 C 0.4966(3) 0.24523(18) 0.79535(14) 0.0345(10) Uani 1 1 d . . . . .
H63A H 0.457536 0.273062 0.816335 0.052 Uiso 1 1 calc GR . . . .
H63B H 0.547282 0.222206 0.820201 0.052 Uiso 1 1 calc GR . . . .
H63C H 0.453574 0.212871 0.774484 0.052 Uiso 1 1 calc GR . . . .
C64 C 0.4347(3) 0.52261(18) 0.69975(13) 0.0265(8) Uani 1 1 d . . . . .
H64 H 0.506362 0.530624 0.699422 0.032 Uiso 1 1 calc R . . . .
C65 C 0.4095(3) 0.5536(2) 0.75127(15) 0.0402(10) Uani 1 1 d . . . . .
H65A H 0.338838 0.548781 0.752429 0.060 Uiso 1 1 calc GR . . . .
H65B H 0.426624 0.600487 0.751916 0.060 Uiso 1 1 calc GR . . . .
H65C H 0.446565 0.531586 0.782877 0.060 Uiso 1 1 calc GR . . . .
C66 C 0.3801(3) 0.5590(2) 0.65103(15) 0.0389(10) Uani 1 1 d . . . . .
H66A H 0.396029 0.539156 0.617462 0.058 Uiso 1 1 calc GR . . . .
H66B H 0.399992 0.605446 0.652584 0.058 Uiso 1 1 calc GR . . . .
H66C H 0.309111 0.555947 0.651653 0.058 Uiso 1 1 calc GR . . . .
O1 O 0.8338(2) 0.72904(17) 0.96707(13) 0.0584(9) Uani 1 1 d . . . . .
C67 C 0.8499(3) 0.6672(2) 0.99276(16) 0.0459(12) Uani 1 1 d . . . . .
H67A H 0.786594 0.647253 0.998789 0.055 Uiso 1 1 calc R . . . .
H67B H 0.892054 0.672074 1.028355 0.055 Uiso 1 1 calc R . . . .
C68 C 0.8999(3) 0.6244(2) 0.95545(15) 0.0433(11) Uani 1 1 d . . . . .
H68A H 0.951250 0.596491 0.976245 0.052 Uiso 1 1 calc R . . . .
H68B H 0.851974 0.595890 0.932734 0.052 Uiso 1 1 calc R . . . .
C69 C 0.9444(3) 0.6743(3) 0.92129(16) 0.0519(13) Uani 1 1 d . . . . .
H69A H 1.008672 0.690328 0.939813 0.062 Uiso 1 1 calc R . . . .
H69B H 0.952758 0.655942 0.885345 0.062 Uiso 1 1 calc R . . . .
C70 C 0.8681(4) 0.7277(3) 0.91620(18) 0.0572(14) Uani 1 1 d . . . . .
H70A H 0.897348 0.770675 0.908489 0.069 Uiso 1 1 calc R . . . .
H70B H 0.813809 0.717571 0.886640 0.069 Uiso 1 1 calc R . . . .
O2 O 0.6896(5) 0.2414(4) 0.4820(3) 0.0510(16) Uani 0.775(10) 1 d . . P A 1
O2B O 0.719(2) 0.2557(15) 0.4941(11) 0.0510(16) Uani 0.225(10) 1 d . . P A 2
C71 C 0.6425(3) 0.3042(2) 0.47770(18) 0.0520(12) Uani 1 1 d . . . . .
H71C H 0.595409 0.290075 0.445818 0.062 Uiso 0.225(10) 1 calc R . P A 2
H71D H 0.669144 0.348388 0.471304 0.062 Uiso 0.225(10) 1 calc R . P A 2
H71A H 0.575587 0.299260 0.457140 0.062 Uiso 0.775(10) 1 calc R . P A 1
H71B H 0.679797 0.334273 0.456885 0.062 Uiso 0.775(10) 1 calc R . P A 1
C72 C 0.6351(5) 0.3337(4) 0.5303(2) 0.0481(18) Uani 0.775(10) 1 d . . P A 1
H72A H 0.569949 0.354324 0.530719 0.058 Uiso 0.775(10) 1 calc R . P A 1
H72B H 0.687063 0.367208 0.540202 0.058 Uiso 0.775(10) 1 calc R . P A 1
C72B C 0.595(2) 0.2993(14) 0.5372(9) 0.0481(18) Uani 0.225(10) 1 d . . P A 2
H72C H 0.594800 0.343062 0.554762 0.058 Uiso 0.225(10) 1 calc R . P A 2
H72D H 0.526945 0.281970 0.530925 0.058 Uiso 0.225(10) 1 calc R . P A 2
C73 C 0.649(2) 0.2753(7) 0.5680(9) 0.064(4) Uani 0.775(10) 1 d . . P A 1
H73A H 0.585699 0.254198 0.571574 0.077 Uiso 0.775(10) 1 calc R . P A 1
H73B H 0.682492 0.288298 0.604446 0.077 Uiso 0.775(10) 1 calc R . P A 1
C73B C 0.657(7) 0.256(3) 0.569(3) 0.064(4) Uani 0.225(10) 1 d . . P A 2
H73C H 0.696207 0.280716 0.598804 0.077 Uiso 0.225(10) 1 calc R . P A 2
H73D H 0.618088 0.222380 0.584370 0.077 Uiso 0.225(10) 1 calc R . P A 2
C74 C 0.7156(4) 0.2284(3) 0.53936(17) 0.0620(15) Uani 1 1 d . . . . .
H74A H 0.786058 0.237830 0.551400 0.074 Uiso 0.775(10) 1 calc R . P A 1
H74B H 0.702496 0.181726 0.547598 0.074 Uiso 0.775(10) 1 calc R . P A 1
H74C H 0.782729 0.227813 0.560161 0.074 Uiso 0.225(10) 1 calc R . P A 2
H74D H 0.694599 0.182005 0.532878 0.074 Uiso 0.225(10) 1 calc R . P A 2
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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 1 0 0.1348
-1 -1 0 0.1093
-1 -1 -1 0.1099
0 0 1 0.0934
0 0 -1 0.1169
1 0 -1 0.1495
1 -1 0 0.0932
0 -1 0 0.1214
0 -1 -1 0.0932
-5 15 29 0.1259
-4 28 0 0.1311
-8 17 26 0.1270
8 -9 -32 0.1053
-1 0 -1 0.1030
1 0 1 0.1336
-17 11 -7 0.0902
1 -1 1 0.0879
-14 19 -2 0.0805
11 -18 16 0.0856
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 Cl1 91.81(9) . . ?
C34 Ge1 Cl1 89.91(9) . . ?
C34 Ge1 C1 92.20(13) . . ?
C2 Ge2 Cl2 91.87(10) . . ?
C35 Ge2 Cl2 89.52(9) . . ?
C35 Ge2 C2 91.89(13) . . ?
C1 N1 C10 125.5(2) . . ?
C3 N1 C1 109.6(3) . . ?
C3 N1 C10 124.8(3) . . ?
C2 N2 C22 124.6(3) . . ?
C3 N2 C2 110.1(2) . . ?
C3 N2 C22 125.3(3) . . ?
C34 N3 C43 124.4(3) . . ?
C36 N3 C34 110.1(2) . . ?
C36 N3 C43 125.2(3) . . ?
C35 N4 C55 123.8(2) . . ?
C36 N4 C35 110.2(3) . . ?
C36 N4 C55 125.8(3) . . ?
N1 C1 Ge1 118.9(2) . . ?
C2 C1 Ge1 134.3(3) . . ?
C2 C1 N1 106.7(3) . . ?
N2 C2 Ge2 121.3(2) . . ?
C1 C2 Ge2 131.5(2) . . ?
C1 C2 N2 106.1(3) . . ?
N1 C3 C4 125.5(3) . . ?
N2 C3 N1 107.4(3) . . ?
N2 C3 C4 127.1(3) . . ?
C5 C4 C3 122.0(3) . . ?
C9 C4 C3 119.5(3) . . ?
C9 C4 C5 118.4(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 C4 120.3(3) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.4(3) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 120.2 . . ?
C8 C7 C6 119.7(3) . . ?
C8 C7 H7 120.2 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.0(3) . . ?
C9 C8 H8 120.0 . . ?
C4 C9 H9 119.4 . . ?
C8 C9 C4 121.3(3) . . ?
C8 C9 H9 119.4 . . ?
C11 C10 N1 119.2(3) . . ?
C11 C10 C15 123.4(3) . . ?
C15 C10 N1 117.3(3) . . ?
C10 C11 C16 123.6(3) . . ?
C12 C11 C10 117.2(3) . . ?
C12 C11 C16 119.2(3) . . ?
C11 C12 H12 119.4 . . ?
C13 C12 C11 121.2(4) . . ?
C13 C12 H12 119.4 . . ?
C12 C13 H13 119.9 . . ?
C12 C13 C14 120.2(4) . . ?
C14 C13 H13 119.9 . . ?
C13 C14 H14 119.5 . . ?
C15 C14 C13 121.0(4) . . ?
C15 C14 H14 119.5 . . ?
C10 C15 C19 123.1(3) . . ?
C14 C15 C10 116.8(3) . . ?
C14 C15 C19 120.1(3) . . ?
C11 C16 H16 108.3 . . ?
C11 C16 C17 111.1(3) . . ?
C11 C16 C18 110.7(3) . . ?
C17 C16 H16 108.3 . . ?
C17 C16 C18 110.0(3) . . ?
C18 C16 H16 108.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C15 C19 H19 107.6 . . ?
C20 C19 C15 111.4(3) . . ?
C20 C19 H19 107.6 . . ?
C21 C19 C15 112.3(3) . . ?
C21 C19 H19 107.6 . . ?
C21 C19 C20 110.1(3) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 N2 118.0(3) . . ?
C23 C22 C27 123.1(3) . . ?
C27 C22 N2 118.9(3) . . ?
C22 C23 C28 124.4(3) . . ?
C24 C23 C22 116.7(3) . . ?
C24 C23 C28 118.9(3) . . ?
C23 C24 H24 119.3 . . ?
C25 C24 C23 121.4(4) . . ?
C25 C24 H24 119.3 . . ?
C24 C25 H25 119.8 . . ?
C24 C25 C26 120.5(3) . . ?
C26 C25 H25 119.8 . . ?
C25 C26 H26 119.6 . . ?
C27 C26 C25 120.8(3) . . ?
C27 C26 H26 119.6 . . ?
C22 C27 C31 122.3(3) . . ?
C26 C27 C22 117.5(3) . . ?
C26 C27 C31 120.1(3) . . ?
C23 C28 H28 107.9 . . ?
C23 C28 C29 111.5(3) . . ?
C23 C28 C30 110.6(3) . . ?
C29 C28 H28 107.9 . . ?
C29 C28 C30 110.9(3) . . ?
C30 C28 H28 107.9 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C31 H31 108.4 . . ?
C32 C31 C27 113.8(3) . . ?
C32 C31 H31 108.4 . . ?
C33 C31 C27 108.6(4) . . ?
C33 C31 H31 108.4 . . ?
C33 C31 C32 109.1(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N3 C34 Ge1 119.9(2) . . ?
C35 C34 Ge1 133.0(2) . . ?
C35 C34 N3 106.5(3) . . ?
N4 C35 Ge2 120.6(2) . . ?
C34 C35 Ge2 131.1(3) . . ?
C34 C35 N4 106.3(3) . . ?
N3 C36 N4 106.9(3) . . ?
N3 C36 C37 127.3(3) . . ?
N4 C36 C37 125.8(3) . . ?
C38 C37 C36 120.9(3) . . ?
C42 C37 C36 120.7(3) . . ?
C42 C37 C38 118.4(3) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 C37 120.4(3) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 119.8 . . ?
C40 C39 C38 120.5(3) . . ?
C40 C39 H39 119.8 . . ?
C39 C40 H40 120.1 . . ?
C39 C40 C41 119.9(3) . . ?
C41 C40 H40 120.1 . . ?
C40 C41 H41 119.8 . . ?
C40 C41 C42 120.4(3) . . ?
C42 C41 H41 119.8 . . ?
C37 C42 H42 119.7 . . ?
C41 C42 C37 120.5(3) . . ?
C41 C42 H42 119.7 . . ?
C44 C43 N3 118.6(3) . . ?
C44 C43 C48 123.4(3) . . ?
C48 C43 N3 118.0(3) . . ?
C43 C44 C49 123.8(3) . . ?
C45 C44 C43 116.6(3) . . ?
C45 C44 C49 119.6(3) . . ?
C44 C45 H45 119.2 . . ?
C46 C45 C44 121.6(3) . . ?
C46 C45 H45 119.2 . . ?
C45 C46 H46 119.6 . . ?
C45 C46 C47 120.7(3) . . ?
C47 C46 H46 119.6 . . ?
C46 C47 H47 119.6 . . ?
C48 C47 C46 120.7(3) . . ?
C48 C47 H47 119.6 . . ?
C43 C48 C52 122.4(3) . . ?
C47 C48 C43 116.7(3) . . ?
C47 C48 C52 120.8(3) . . ?
C44 C49 H49 107.9 . . ?
C44 C49 C50 110.7(3) . . ?
C44 C49 C51 112.3(3) . . ?
C50 C49 H49 107.9 . . ?
C51 C49 H49 107.9 . . ?
C51 C49 C50 109.9(3) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51B 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C48 C52 H52 107.1 . . ?
C53 C52 C48 112.6(3) . . ?
C53 C52 H52 107.1 . . ?
C53 C52 C54 109.6(3) . . ?
C54 C52 C48 113.1(3) . . ?
C54 C52 H52 107.1 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C55 N4 119.3(3) . . ?
C56 C55 C60 123.1(3) . . ?
C60 C55 N4 117.6(3) . . ?
C55 C56 C61 122.8(3) . . ?
C57 C56 C55 116.9(3) . . ?
C57 C56 C61 120.3(3) . . ?
C56 C57 H57 119.3 . . ?
C58 C57 C56 121.3(4) . . ?
C58 C57 H57 119.3 . . ?
C57 C58 H58 120.0 . . ?
C57 C58 C59 120.0(3) . . ?
C59 C58 H58 120.0 . . ?
C58 C59 H59 119.1 . . ?
C58 C59 C60 121.7(4) . . ?
C60 C59 H59 119.1 . . ?
C55 C60 C64 121.9(3) . . ?
C59 C60 C55 116.8(3) . . ?
C59 C60 C64 121.3(3) . . ?
C56 C61 H61 107.7 . . ?
C56 C61 C62 110.9(3) . . ?
C56 C61 C63 112.4(3) . . ?
C62 C61 H61 107.7 . . ?
C63 C61 H61 107.7 . . ?
C63 C61 C62 110.4(3) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62B 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63B 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C60 C64 H64 106.7 . . ?
C65 C64 C60 114.3(3) . . ?
C65 C64 H64 106.7 . . ?
C65 C64 C66 109.0(3) . . ?
C66 C64 C60 113.0(3) . . ?
C66 C64 H64 106.7 . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C67 O1 C70 109.7(3) . . ?
O1 C67 H67A 110.4 . . ?
O1 C67 H67B 110.4 . . ?
O1 C67 C68 106.8(3) . . ?
H67A C67 H67B 108.6 . . ?
C68 C67 H67A 110.4 . . ?
C68 C67 H67B 110.4 . . ?
C67 C68 H68A 111.2 . . ?
C67 C68 H68B 111.2 . . ?
H68A C68 H68B 109.1 . . ?
C69 C68 C67 102.7(4) . . ?
C69 C68 H68A 111.2 . . ?
C69 C68 H68B 111.2 . . ?
C68 C69 H69A 111.5 . . ?
C68 C69 H69B 111.5 . . ?
H69A C69 H69B 109.3 . . ?
C70 C69 C68 101.4(4) . . ?
C70 C69 H69A 111.5 . . ?
C70 C69 H69B 111.5 . . ?
O1 C70 C69 105.0(4) . . ?
O1 C70 H70A 110.8 . . ?
O1 C70 H70B 110.8 . . ?
C69 C70 H70A 110.8 . . ?
C69 C70 H70B 110.8 . . ?
H70A C70 H70B 108.8 . . ?
C71 O2 C74 106.4(5) . . ?
C74 O2B C71 115(2) . . ?
O2 C71 H71A 109.0 . . ?
O2 C71 H71B 109.0 . . ?
O2 C71 C72 113.0(5) . . ?
O2B C71 H71C 112.9 . . ?
O2B C71 H71D 112.9 . . ?
O2B C71 C72B 94.0(15) . . ?
H71C C71 H71D 110.4 . . ?
H71A C71 H71B 107.8 . . ?
C72 C71 H71A 109.0 . . ?
C72 C71 H71B 109.0 . . ?
C72B C71 H71C 112.9 . . ?
C72B C71 H71D 112.9 . . ?
C71 C72 H72A 111.3 . . ?
C71 C72 H72B 111.3 . . ?
C71 C72 C73 102.4(8) . . ?
H72A C72 H72B 109.2 . . ?
C73 C72 H72A 111.3 . . ?
C73 C72 H72B 111.3 . . ?
C71 C72B H72C 110.9 . . ?
C71 C72B H72D 110.9 . . ?
H72C C72B H72D 109.0 . . ?
C73B C72B C71 104(4) . . ?
C73B C72B H72C 110.9 . . ?
C73B C72B H72D 110.9 . . ?
C72 C73 H73A 111.1 . . ?
C72 C73 H73B 111.1 . . ?
C72 C73 C74 103.3(14) . . ?
H73A C73 H73B 109.1 . . ?
C74 C73 H73A 111.1 . . ?
C74 C73 H73B 111.1 . . ?
C72B C73B H73C 109.6 . . ?
C72B C73B H73D 109.6 . . ?
H73C C73B H73D 108.1 . . ?
C74 C73B C72B 110(6) . . ?
C74 C73B H73C 109.6 . . ?
C74 C73B H73D 109.6 . . ?
O2 C74 C73 105.1(9) . . ?
O2 C74 H74A 110.7 . . ?
O2 C74 H74B 110.7 . . ?
O2B C74 C73B 115(4) . . ?
O2B C74 H74C 108.6 . . ?
O2B C74 H74D 108.6 . . ?
C73 C74 H74A 110.7 . . ?
C73 C74 H74B 110.7 . . ?
C73B C74 H74C 108.6 . . ?
C73B C74 H74D 108.6 . . ?
H74A C74 H74B 108.8 . . ?
H74C C74 H74D 107.6 . . ?
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 Cl1 2.3329(10) . ?
Ge1 C1 2.027(3) . ?
Ge1 C34 2.021(3) . ?
Ge2 Cl2 2.3410(11) . ?
Ge2 C2 2.033(3) . ?
Ge2 C35 2.032(3) . ?
N1 C1 1.411(4) . ?
N1 C3 1.352(4) . ?
N1 C10 1.455(4) . ?
N2 C2 1.421(4) . ?
N2 C3 1.332(4) . ?
N2 C22 1.452(4) . ?
N3 C34 1.410(4) . ?
N3 C36 1.340(4) . ?
N3 C43 1.453(4) . ?
N4 C35 1.402(4) . ?
N4 C36 1.350(4) . ?
N4 C55 1.449(4) . ?
C1 C2 1.362(4) . ?
C3 C4 1.487(4) . ?
C4 C5 1.395(5) . ?
C4 C9 1.391(4) . ?
C5 H5 0.9500 . ?
C5 C6 1.389(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.384(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.381(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.380(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.397(5) . ?
C10 C15 1.400(5) . ?
C11 C12 1.388(5) . ?
C11 C16 1.523(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.373(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.398(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.386(5) . ?
C15 C19 1.525(5) . ?
C16 H16 1.0000 . ?
C16 C17 1.535(5) . ?
C16 C18 1.538(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19 1.0000 . ?
C19 C20 1.523(5) . ?
C19 C21 1.520(5) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.399(5) . ?
C22 C27 1.400(5) . ?
C23 C24 1.393(4) . ?
C23 C28 1.511(5) . ?
C24 H24 0.9500 . ?
C24 C25 1.375(5) . ?
C25 H25 0.9500 . ?
C25 C26 1.387(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.382(5) . ?
C27 C31 1.547(5) . ?
C28 H28 1.0000 . ?
C28 C29 1.528(5) . ?
C28 C30 1.534(5) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31 1.0000 . ?
C31 C32 1.521(6) . ?
C31 C33 1.516(6) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.367(4) . ?
C36 C37 1.482(4) . ?
C37 C38 1.402(5) . ?
C37 C42 1.391(5) . ?
C38 H38 0.9500 . ?
C38 C39 1.384(5) . ?
C39 H39 0.9500 . ?
C39 C40 1.374(5) . ?
C40 H40 0.9500 . ?
C40 C41 1.377(5) . ?
C41 H41 0.9500 . ?
C41 C42 1.387(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.406(4) . ?
C43 C48 1.412(5) . ?
C44 C45 1.396(4) . ?
C44 C49 1.511(5) . ?
C45 H45 0.9500 . ?
C45 C46 1.370(5) . ?
C46 H46 0.9500 . ?
C46 C47 1.397(5) . ?
C47 H47 0.9500 . ?
C47 C48 1.395(4) . ?
C48 C52 1.528(4) . ?
C49 H49 1.0000 . ?
C49 C50 1.538(5) . ?
C49 C51 1.531(5) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52 1.0000 . ?
C52 C53 1.516(5) . ?
C52 C54 1.527(5) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.401(5) . ?
C55 C60 1.408(5) . ?
C56 C57 1.397(5) . ?
C56 C61 1.511(5) . ?
C57 H57 0.9500 . ?
C57 C58 1.381(5) . ?
C58 H58 0.9500 . ?
C58 C59 1.383(5) . ?
C59 H59 0.9500 . ?
C59 C60 1.386(5) . ?
C60 C64 1.532(5) . ?
C61 H61 1.0000 . ?
C61 C62 1.540(5) . ?
C61 C63 1.536(5) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64 1.0000 . ?
C64 C65 1.512(5) . ?
C64 C66 1.520(5) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
O1 C67 1.411(5) . ?
O1 C70 1.413(5) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C67 C68 1.507(6) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C68 C69 1.506(6) . ?
C69 H69A 0.9900 . ?
C69 H69B 0.9900 . ?
C69 C70 1.501(7) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
O2 C71 1.425(8) . ?
O2 C74 1.445(8) . ?
O2B C71 1.45(3) . ?
O2B C74 1.26(3) . ?
C71 H71C 0.9900 . ?
C71 H71D 0.9900 . ?
C71 H71A 0.9900 . ?
C71 H71B 0.9900 . ?
C71 C72 1.456(7) . ?
C71 C72B 1.70(2) . ?
C72 H72A 0.9900 . ?
C72 H72B 0.9900 . ?
C72 C73 1.505(18) . ?
C72B H72C 0.9900 . ?
C72B H72D 0.9900 . ?
C72B C73B 1.38(8) . ?
C73 H73A 0.9900 . ?
C73 H73B 0.9900 . ?
C73 C74 1.56(2) . ?
C73B H73C 0.9900 . ?
C73B H73D 0.9900 . ?
C73B C74 1.29(8) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C74 H74C 0.9900 . ?
C74 H74D 0.9900 . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7880 89614 190061 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.2120 0 190061 nmt -1.0091 -0.0072 -0.0382 -0.0126 0.9993 0.0137 0.1288
0.0261 -0.9872
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
0.9994 0.9991 0.0020 0.0565 -0.0238 0.0135
-0.9994 -0.9991 -0.0020 -0.0565 0.0238 -0.0135
-0.9988 -0.9987 -1.0018 -0.0671 0.0231 0.0133
-0.0007 -0.0004 0.9997 0.0106 0.0007 -0.0268
0.0007 0.0004 -0.9997 -0.0106 -0.0007 0.0268
0.9998 -0.0002 -0.9972 0.0392 0.0097 0.0385
0.9989 -1.0003 0.0030 0.0429 0.0447 0.0099
-0.0003 -0.9997 0.0005 -0.0068 0.0342 -0.0018
0.0004 -0.9993 -0.9993 -0.0173 0.0335 0.0250
-4.9595 15.3103 29.2252 0.1667 -0.5556 -0.8146
-4.3274 27.8769 0.0791 -0.0254 -0.9997 -0.0035
-8.1568 16.7234 26.2060 -0.0148 -0.6393 -0.7688
8.1181 -8.8746 -31.7335 0.0075 0.3663 0.9305
-0.9985 0.0010 -1.0022 -0.0603 -0.0111 0.0151
0.9985 -0.0010 1.0022 0.0603 0.0111 -0.0151
-16.6404 11.3578 -6.8879 -0.8236 -0.5670 0.0090
0.9982 -1.0007 1.0027 0.0535 0.0454 -0.0169
-14.2440 18.7412 -2.3901 -0.6067 -0.7918 -0.0702
10.5963 -18.2932 15.9800 0.5723 0.7480 -0.3362
