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#$Date: 2025-08-22 10:56:18 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301860 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/38/7123868.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_7123868
loop_
_publ_author_name
'Chen, Xiao'
'Simler, Thomas'
'Yadav, Ravi'
'Gamer, Michael T.'
'Köppe, Ralf'
'Roesky, Peter W.'
_publ_section_title
;
 Reaction of an arsinoamide with chloro tetrylenes: substitution and As--N
 bond insertion
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04530A
_journal_year                    2019
_chemical_formula_moiety         'C48 H54 As2 Ge N2'
_chemical_formula_sum            'C48 H54 As2 Ge N2'
_chemical_formula_weight         881.36
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-12 deposited with the CCDC.    2019-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.787(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0143(7)
_cell_length_b                   18.0257(7)
_cell_length_c                   19.1618(10)
_cell_measurement_reflns_used    12144
_cell_measurement_temperature    210
_cell_measurement_theta_max      29.32
_cell_measurement_theta_min      1.99
_cell_volume                     4280.3(4)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_molecular_graphics    'Diamond 4, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
MS Word (Microsoft)
Olex2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      210
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14395
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.496
_diffrn_reflns_theta_min         1.994
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_diffrn_source_current           40mA
_diffrn_source_power             2kW
_diffrn_source_voltage           50kV
_exptl_absorpt_coefficient_mu    2.284
_exptl_absorpt_correction_T_max  0.7007
_exptl_absorpt_correction_T_min  0.4074
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       rod
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0621P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4535
_reflns_number_total             5950
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc04530a2.cif
_cod_data_source_block           xcd150
_cod_database_code               7123868
_shelx_shelxl_version_number     2018/3
_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   0.851
_shelx_estimated_absorpt_t_min   0.653
_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 Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C12(H12), C14(H14), C20(H20), C21(H21), C22(H22), C23(H23),
 C24(H24)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'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, -y, -z'
'x, -y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
As As 0.33929(2) 0.73581(2) 0.34450(2) 0.03289(8) Uani 1 1 d . . .
Ge Ge 0.500000 0.78627(2) 0.250000 0.03681(11) Uani 1 2 d S T P
N N 0.46145(16) 0.72017(12) 0.31358(13) 0.0327(4) Uani 1 1 d . . .
C1 C 0.25508(19) 0.79365(16) 0.25724(15) 0.0358(5) Uani 1 1 d . . .
C2 C 0.2716(2) 0.86822(17) 0.24050(16) 0.0399(6) Uani 1 1 d . . .
C3 C 0.2158(2) 0.8950(2) 0.17101(17) 0.0492(7) Uani 1 1 d . . .
H3 H 0.227969 0.943617 0.159457 0.059 Uiso 1 1 calc R . .
C4 C 0.1428(2) 0.8523(2) 0.11814(17) 0.0530(8) Uani 1 1 d . . .
C5 C 0.1226(2) 0.7811(2) 0.13709(18) 0.0511(8) Uani 1 1 d . . .
H5 H 0.072092 0.752190 0.103176 0.061 Uiso 1 1 calc R . .
C6 C 0.1762(2) 0.75137(18) 0.20587(17) 0.0434(6) Uani 1 1 d . . .
C7 C 0.1459(2) 0.6735(2) 0.2217(2) 0.0554(8) Uani 1 1 d . . .
H7A H 0.205694 0.640738 0.225947 0.083 Uiso 1 1 calc GR . .
H7B H 0.084722 0.657055 0.182490 0.083 Uiso 1 1 calc GR . .
H7C H 0.128169 0.673268 0.266812 0.083 Uiso 1 1 calc GR . .
C8 C 0.0866(3) 0.8838(3) 0.0425(2) 0.0773(13) Uani 1 1 d . . .
H8A H 0.051816 0.929588 0.047337 0.116 Uiso 1 1 calc GR . .
H8B H 0.033693 0.849006 0.015123 0.116 Uiso 1 1 calc GR . .
H8C H 0.138854 0.892600 0.017289 0.116 Uiso 1 1 calc GR . .
C9 C 0.3450(2) 0.92217(17) 0.29287(19) 0.0472(7) Uani 1 1 d . . .
H9A H 0.310606 0.939296 0.327611 0.071 Uiso 1 1 calc GR . .
H9B H 0.359626 0.963659 0.265928 0.071 Uiso 1 1 calc GR . .
H9C H 0.411559 0.897869 0.318356 0.071 Uiso 1 1 calc GR . .
C10 C 0.3727(2) 0.81110(15) 0.42339(15) 0.0347(5) Uani 1 1 d . . .
C11 C 0.4740(2) 0.84010(16) 0.46441(16) 0.0404(6) Uani 1 1 d . . .
C12 C 0.4787(2) 0.89048(18) 0.51989(18) 0.0492(7) Uani 1 1 d . . .
H12 H 0.545454 0.910522 0.545451 0.059 Uiso 1 1 calc R . .
C13 C 0.3891(3) 0.91253(18) 0.53926(18) 0.0498(7) Uani 1 1 d . . .
C14 C 0.2905(2) 0.88165(18) 0.50049(17) 0.0464(7) Uani 1 1 d . . .
H14 H 0.229404 0.894526 0.513252 0.056 Uiso 1 1 calc R . .
C15 C 0.2802(2) 0.83211(16) 0.44322(16) 0.0387(6) Uani 1 1 d . . .
C16 C 0.1688(2) 0.80214(18) 0.40375(19) 0.0485(7) Uani 1 1 d . . .
H16A H 0.145428 0.820809 0.354485 0.073 Uiso 1 1 calc GR . .
H16B H 0.119129 0.817700 0.429000 0.073 Uiso 1 1 calc GR . .
H16C H 0.171264 0.748936 0.402774 0.073 Uiso 1 1 calc GR . .
C17 C 0.3982(4) 0.9673(3) 0.6003(2) 0.0749(12) Uani 1 1 d . . .
H17A H 0.348501 1.007400 0.582542 0.112 Uiso 1 1 calc GR . .
H17B H 0.470414 0.986435 0.617227 0.112 Uiso 1 1 calc GR . .
H17C H 0.381360 0.942973 0.640040 0.112 Uiso 1 1 calc GR . .
C18 C 0.5787(2) 0.8195(2) 0.45037(19) 0.0512(8) Uani 1 1 d . . .
H18A H 0.583099 0.766538 0.446729 0.077 Uiso 1 1 calc GR . .
H18B H 0.638450 0.837028 0.490069 0.077 Uiso 1 1 calc GR . .
H18C H 0.581038 0.841843 0.405397 0.077 Uiso 1 1 calc GR . .
C19 C 0.51370(19) 0.65046(14) 0.33343(14) 0.0331(5) Uani 1 1 d . . .
C20 C 0.4579(2) 0.58349(16) 0.32704(17) 0.0418(6) Uani 1 1 d . . .
H20 H 0.382805 0.583760 0.311568 0.050 Uiso 1 1 calc R . .
C21 C 0.5123(3) 0.51664(18) 0.3433(2) 0.0527(8) Uani 1 1 d . . .
H21 H 0.473596 0.472593 0.338814 0.063 Uiso 1 1 calc R . .
C22 C 0.6238(3) 0.5150(2) 0.3663(2) 0.0566(8) Uani 1 1 d . . .
H22 H 0.660267 0.469969 0.376812 0.068 Uiso 1 1 calc R . .
C23 C 0.6807(2) 0.5807(2) 0.37360(18) 0.0512(8) Uani 1 1 d . . .
H23 H 0.755786 0.579814 0.389191 0.061 Uiso 1 1 calc R . .
C24 C 0.6268(2) 0.64804(17) 0.35781(16) 0.0404(6) Uani 1 1 d . . .
H24 H 0.666092 0.691936 0.363441 0.048 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'
As As 0.0499 2.0058 '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'
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_3
N As C1 96.63(10) .
N As C10 109.50(10) .
C10 As C1 102.63(11) .
N Ge N 101.27(13) 2_655
Ge N As 121.90(11) .
C19 N As 115.41(16) .
C19 N Ge 122.17(15) .
C2 C1 As 127.3(2) .
C6 C1 As 113.6(2) .
C6 C1 C2 119.0(3) .
C1 C2 C9 124.8(3) .
C3 C2 C1 118.3(3) .
C3 C2 C9 116.8(3) .
C4 C3 C2 123.1(3) .
C3 C4 C8 120.7(4) .
C5 C4 C3 117.7(3) .
C5 C4 C8 121.5(4) .
C4 C5 C6 121.6(3) .
C1 C6 C7 122.7(3) .
C5 C6 C1 119.9(3) .
C5 C6 C7 117.4(3) .
C11 C10 As 129.00(19) .
C11 C10 C15 118.4(2) .
C15 C10 As 112.38(19) .
C10 C11 C18 123.2(3) .
C12 C11 C10 119.0(2) .
C12 C11 C18 117.8(3) .
C11 C12 C13 123.4(3) .
C12 C13 C14 117.3(3) .
C12 C13 C17 121.5(3) .
C14 C13 C17 121.2(3) .
C13 C14 C15 122.1(3) .
C10 C15 C16 122.1(3) .
C14 C15 C10 119.8(3) .
C14 C15 C16 118.0(2) .
C20 C19 N 123.1(2) .
C20 C19 C24 117.9(2) .
C24 C19 N 118.9(2) .
C21 C20 C19 121.1(3) .
C22 C21 C20 120.4(3) .
C23 C22 C21 119.5(3) .
C22 C23 C24 120.5(3) .
C23 C24 C19 120.6(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
As N 1.8797(19) .
As C1 1.991(3) .
As C10 1.979(3) .
Ge N 1.879(2) 2_655
Ge N 1.879(2) .
N C19 1.424(3) .
C1 C2 1.414(4) .
C1 C6 1.409(4) .
C2 C3 1.394(4) .
C2 C9 1.510(4) .
C3 C4 1.390(5) .
C4 C5 1.381(5) .
C4 C8 1.520(5) .
C5 C6 1.396(5) .
C6 C7 1.514(5) .
C10 C11 1.412(4) .
C10 C15 1.420(3) .
C11 C12 1.385(4) .
C11 C18 1.514(4) .
C12 C13 1.385(4) .
C13 C14 1.388(5) .
C13 C17 1.508(5) .
C14 C15 1.389(4) .
C15 C16 1.515(4) .
C19 C20 1.395(4) .
C19 C24 1.403(3) .
C20 C21 1.384(4) .
C21 C22 1.383(5) .
C22 C23 1.381(5) .
C23 C24 1.389(4) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168350840
