# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
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data_xcd310
_database_code_depnum_ccdc_archive 'CCDC 1922573'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record
;
2019-06-12 deposited with the CCDC. 2019-07-05 downloaded from the CCDC.
;
_audit_creation_date 2019-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
#==============================================================================
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C39 H50 As N3 Si'
_chemical_formula_sum 'C39 H50 As N3 Si'
_chemical_formula_weight 663.83
_chemical_melting_point ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
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'
_cell_length_a 16.8814(4)
_cell_length_b 12.7921(3)
_cell_length_c 18.4683(5)
_cell_angle_alpha 90
_cell_angle_beta 116.297(2)
_cell_angle_gamma 90
_cell_volume 3575.46(16)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 34165
_cell_measurement_temperature 150
_cell_measurement_theta_max 29.64
_cell_measurement_theta_min 2.01
_shelx_estimated_absorpt_T_max 0.813
_shelx_estimated_absorpt_T_min 0.691
_exptl_absorpt_coefficient_mu 1.015
_exptl_absorpt_correction_T_max 0.7781
_exptl_absorpt_correction_T_min 0.4204
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens published in F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol.9, no.2, 2016, pp. 136-140.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.233
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description irregular
_exptl_crystal_F_000 1408
_exptl_crystal_size_max 0.393
_exptl_crystal_size_mid 0.324
_exptl_crystal_size_min 0.213
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0350
_diffrn_reflns_av_unetI/netI 0.0365
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 28628
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 29.228
_diffrn_reflns_theta_min 2.012
_diffrn_ambient_temperature 150
_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 0.992
_diffrn_measurement_details
;
235 frames, detector distance = 100 mm
;
_diffrn_measurement_device '2-circle diffractometer'
_diffrn_measurement_device_type 'STOE IPDS II'
_diffrn_measurement_method 'rotation method, \w 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_source 'sealed tube, 12x0.4mm long-fine focus'
_diffrn_source_current 40mA
_diffrn_source_power 2kW
_diffrn_source_target ?
_diffrn_source_type ?
_diffrn_source_voltage 50kV
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7412
_reflns_number_total 9644
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_data_collection 'STOE X-AREA'
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_structure_solution 'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)'
_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)
;
_refine_diff_density_max 0.906
_refine_diff_density_min -0.433
_refine_diff_density_rms 0.075
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.014
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 409
_refine_ls_number_reflns 9644
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0612
_refine_ls_R_factor_gt 0.0432
_refine_ls_restrained_S_all 1.014
_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/[\s^2^(Fo^2^)+(0.0819P)^2^+0.1514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1126
_refine_ls_wR_factor_ref 0.1222
_refine_special_details ?
_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), C21(H21), C22(H22), C23(H23), C24(H24),
C25(H25), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
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), C27(H27A,H27B,H27C), C28(H28A,H28B,
H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
H33B,H33C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
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
As As 0.68248(2) 0.64498(2) 0.34231(2) 0.02755(7) Uani 1 1 d . . . . .
Si Si 0.79785(4) 0.67521(4) 0.30280(3) 0.02748(12) Uani 1 1 d . . . . .
N1 N 0.85063(11) 0.78954(13) 0.36636(10) 0.0279(3) Uani 1 1 d . . . . .
N2 N 0.75238(11) 0.79352(14) 0.24261(10) 0.0310(3) Uani 1 1 d . . . . .
N3 N 0.85813(14) 0.60145(16) 0.28057(12) 0.0430(4) Uani 1 1 d . . . . .
C1 C 0.68880(13) 0.51887(15) 0.40781(11) 0.0285(4) Uani 1 1 d . . . . .
C2 C 0.75897(14) 0.44883(16) 0.44485(12) 0.0323(4) Uani 1 1 d . . . . .
C3 C 0.75433(16) 0.37231(17) 0.49741(13) 0.0372(5) Uani 1 1 d . . . . .
H3 H 0.802671 0.325692 0.522807 0.045 Uiso 1 1 calc R . . . .
C4 C 0.68274(16) 0.36217(17) 0.51357(13) 0.0372(5) Uani 1 1 d . . . . .
C5 C 0.61219(15) 0.42968(17) 0.47379(12) 0.0346(4) Uani 1 1 d . . . . .
H5 H 0.560533 0.421320 0.481517 0.041 Uiso 1 1 calc R . . . .
C6 C 0.61410(13) 0.50896(16) 0.42315(11) 0.0304(4) Uani 1 1 d . . . . .
C7 C 0.53574(14) 0.58205(19) 0.38839(13) 0.0375(5) Uani 1 1 d . . . . .
H7A H 0.556564 0.654588 0.397020 0.056 Uiso 1 1 calc GR . . . .
H7B H 0.497824 0.570072 0.415241 0.056 Uiso 1 1 calc GR . . . .
H7C H 0.502015 0.568886 0.330357 0.056 Uiso 1 1 calc GR . . . .
C8 C 0.6787(2) 0.2824(2) 0.57208(16) 0.0514(6) Uani 1 1 d . . . . .
H8A H 0.729927 0.235794 0.589520 0.077 Uiso 1 1 calc GR . . . .
H8B H 0.624300 0.241355 0.545513 0.077 Uiso 1 1 calc GR . . . .
H8C H 0.679228 0.318271 0.619179 0.077 Uiso 1 1 calc GR . . . .
C9 C 0.84139(14) 0.44835(18) 0.43226(14) 0.0378(5) Uani 1 1 d . . . . .
H9A H 0.831306 0.489925 0.384382 0.057 Uiso 1 1 calc GR . . . .
H9B H 0.855894 0.376320 0.424519 0.057 Uiso 1 1 calc GR . . . .
H9C H 0.890516 0.478492 0.479716 0.057 Uiso 1 1 calc GR . . . .
C10 C 0.58562(12) 0.60228(16) 0.23762(11) 0.0281(4) Uani 1 1 d . . . . .
C11 C 0.58545(13) 0.50686(16) 0.19928(12) 0.0305(4) Uani 1 1 d . . . . .
C12 C 0.51132(15) 0.48047(18) 0.12864(13) 0.0365(4) Uani 1 1 d . . . . .
H12 H 0.510885 0.415705 0.103294 0.044 Uiso 1 1 calc R . . . .
C13 C 0.43806(14) 0.5451(2) 0.09381(13) 0.0399(5) Uani 1 1 d . . . . .
C14 C 0.44075(15) 0.64062(19) 0.13092(13) 0.0378(5) Uani 1 1 d . . . . .
H14 H 0.391786 0.686724 0.107095 0.045 Uiso 1 1 calc R . . . .
C15 C 0.51297(14) 0.67056(17) 0.20181(12) 0.0319(4) Uani 1 1 d . . . . .
C16 C 0.50880(15) 0.77559(18) 0.23763(14) 0.0399(5) Uani 1 1 d . . . . .
H16A H 0.491919 0.765617 0.281554 0.060 Uiso 1 1 calc GR . . . .
H16B H 0.464911 0.819858 0.195734 0.060 Uiso 1 1 calc GR . . . .
H16C H 0.566871 0.809317 0.258801 0.060 Uiso 1 1 calc GR . . . .
C17 C 0.35831(17) 0.5125(2) 0.01769(15) 0.0553(7) Uani 1 1 d . . . . .
H17A H 0.374059 0.510188 -0.027375 0.083 Uiso 1 1 calc GR . . . .
H17B H 0.310512 0.563110 0.005655 0.083 Uiso 1 1 calc GR . . . .
H17C H 0.338676 0.443137 0.025461 0.083 Uiso 1 1 calc GR . . . .
C18 C 0.66227(14) 0.43214(17) 0.23069(13) 0.0362(4) Uani 1 1 d . . . . .
H18A H 0.715264 0.468038 0.234511 0.054 Uiso 1 1 calc GR . . . .
H18B H 0.649034 0.372618 0.193733 0.054 Uiso 1 1 calc GR . . . .
H18C H 0.672521 0.407101 0.284286 0.054 Uiso 1 1 calc GR . . . .
C19 C 0.80349(13) 0.85411(15) 0.30555(12) 0.0289(4) Uani 1 1 d . . . . .
C20 C 0.80827(14) 0.97021(16) 0.30649(12) 0.0326(4) Uani 1 1 d . . . . .
C21 C 0.74410(16) 1.03098(19) 0.31384(15) 0.0435(5) Uani 1 1 d . . . . .
H21 H 0.697050 0.998880 0.320580 0.052 Uiso 1 1 calc R . . . .
C22 C 0.7493(2) 1.1394(2) 0.31124(17) 0.0508(6) Uani 1 1 d . . . . .
H22 H 0.706160 1.181369 0.317208 0.061 Uiso 1 1 calc R . . . .
C23 C 0.81637(19) 1.18638(19) 0.30013(15) 0.0498(6) Uani 1 1 d . . . . .
H23 H 0.818825 1.260402 0.297517 0.060 Uiso 1 1 calc R . . . .
C24 C 0.88000(18) 1.12595(18) 0.29279(15) 0.0451(6) Uani 1 1 d . . . . .
H24 H 0.926300 1.158571 0.285156 0.054 Uiso 1 1 calc R . . . .
C25 C 0.87691(15) 1.01783(17) 0.29648(13) 0.0377(5) Uani 1 1 d . . . . .
H25 H 0.921394 0.976496 0.292191 0.045 Uiso 1 1 calc R . . . .
C26 C 0.90644(13) 0.81062(16) 0.45334(11) 0.0305(4) Uani 1 1 d . . . . .
C27 C 0.85929(18) 0.8805(2) 0.48900(15) 0.0469(6) Uani 1 1 d . . . . .
H27A H 0.850582 0.950113 0.464519 0.070 Uiso 1 1 calc GR . . . .
H27B H 0.895237 0.886262 0.547515 0.070 Uiso 1 1 calc GR . . . .
H27C H 0.801788 0.849945 0.477867 0.070 Uiso 1 1 calc GR . . . .
C28 C 0.99458(16) 0.8576(2) 0.46557(15) 0.0456(6) Uani 1 1 d . . . . .
H28A H 1.033172 0.865148 0.523486 0.068 Uiso 1 1 calc GR . . . .
H28B H 0.984419 0.926388 0.439608 0.068 Uiso 1 1 calc GR . . . .
H28C H 1.022765 0.811484 0.441462 0.068 Uiso 1 1 calc GR . . . .
C29 C 0.92452(16) 0.70414(19) 0.49488(13) 0.0425(5) Uani 1 1 d . . . . .
H29A H 0.869187 0.674905 0.491168 0.064 Uiso 1 1 calc GR . . . .
H29B H 0.966763 0.712241 0.551806 0.064 Uiso 1 1 calc GR . . . .
H29C H 0.949212 0.656915 0.468322 0.064 Uiso 1 1 calc GR . . . .
C30 C 0.70916(14) 0.81926(18) 0.15463(12) 0.0343(4) Uani 1 1 d . . . . .
C31 C 0.64209(19) 0.9070(2) 0.13594(15) 0.0545(7) Uani 1 1 d . . . . .
H31A H 0.603083 0.891593 0.161134 0.082 Uiso 1 1 calc GR . . . .
H31B H 0.606884 0.912853 0.077338 0.082 Uiso 1 1 calc GR . . . .
H31C H 0.673110 0.973018 0.157324 0.082 Uiso 1 1 calc GR . . . .
C32 C 0.77826(18) 0.8462(3) 0.12643(15) 0.0558(7) Uani 1 1 d . . . . .
H32A H 0.806819 0.912315 0.150993 0.084 Uiso 1 1 calc GR . . . .
H32B H 0.750022 0.853123 0.067482 0.084 Uiso 1 1 calc GR . . . .
H32C H 0.822689 0.790509 0.142535 0.084 Uiso 1 1 calc GR . . . .
C33 C 0.65944(18) 0.7211(2) 0.11043(13) 0.0483(6) Uani 1 1 d . . . . .
H33A H 0.700406 0.661816 0.125295 0.072 Uiso 1 1 calc GR . . . .
H33B H 0.634138 0.732542 0.051984 0.072 Uiso 1 1 calc GR . . . .
H33C H 0.611923 0.706041 0.125694 0.072 Uiso 1 1 calc GR . . . .
C34 C 0.88786(13) 0.51650(16) 0.25663(12) 0.0306(4) Uani 1 1 d . . . . .
C35 C 0.95673(15) 0.4530(2) 0.31058(14) 0.0408(5) Uani 1 1 d . . . . .
H35 H 0.984590 0.470008 0.366417 0.049 Uiso 1 1 calc R . . . .
C36 C 0.98488(16) 0.36476(19) 0.28313(16) 0.0439(6) Uani 1 1 d . . . . .
H36 H 1.030456 0.322071 0.320996 0.053 Uiso 1 1 calc R . . . .
C37 C 0.94821(19) 0.3391(2) 0.20333(18) 0.0486(6) Uani 1 1 d . . . . .
H37 H 0.968007 0.279245 0.185555 0.058 Uiso 1 1 calc R . . . .
C38 C 0.88261(17) 0.4006(2) 0.14927(16) 0.0481(6) Uani 1 1 d . . . . .
H38 H 0.857317 0.383793 0.093407 0.058 Uiso 1 1 calc R . . . .
C39 C 0.85241(15) 0.4870(2) 0.17466(14) 0.0405(5) Uani 1 1 d . . . . .
H39 H 0.806269 0.527880 0.135583 0.049 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As 0.03142(11) 0.02188(11) 0.02747(11) -0.00148(7) 0.01133(8) -0.00186(7)
Si 0.0330(3) 0.0223(3) 0.0249(2) 0.00066(19) 0.0108(2) -0.0004(2)
N1 0.0330(8) 0.0225(8) 0.0268(7) 0.0001(6) 0.0119(6) -0.0023(6)
N2 0.0380(9) 0.0259(8) 0.0260(8) 0.0038(6) 0.0112(7) 0.0023(7)
N3 0.0566(12) 0.0320(10) 0.0487(11) 0.0008(9) 0.0309(10) 0.0034(9)
C1 0.0368(10) 0.0225(9) 0.0248(8) -0.0013(7) 0.0124(8) -0.0036(7)
C2 0.0376(10) 0.0273(10) 0.0298(9) -0.0017(8) 0.0129(8) -0.0019(8)
C3 0.0471(12) 0.0297(11) 0.0327(10) 0.0028(8) 0.0158(9) 0.0046(9)
C4 0.0527(13) 0.0302(11) 0.0294(10) 0.0005(8) 0.0189(9) -0.0027(9)
C5 0.0437(11) 0.0342(11) 0.0280(9) -0.0032(8) 0.0179(8) -0.0060(9)
C6 0.0369(10) 0.0287(10) 0.0263(9) -0.0031(7) 0.0146(8) -0.0032(8)
C7 0.0383(11) 0.0422(13) 0.0354(10) 0.0044(9) 0.0195(9) 0.0012(9)
C8 0.0733(17) 0.0410(14) 0.0464(13) 0.0122(11) 0.0326(13) 0.0014(12)
C9 0.0411(11) 0.0299(11) 0.0422(11) 0.0060(9) 0.0184(9) 0.0041(8)
C10 0.0308(9) 0.0268(9) 0.0260(8) 0.0014(7) 0.0118(7) -0.0025(7)
C11 0.0353(10) 0.0268(10) 0.0308(9) 0.0002(8) 0.0160(8) -0.0030(7)
C12 0.0440(12) 0.0318(11) 0.0327(10) -0.0034(8) 0.0161(9) -0.0074(9)
C13 0.0349(11) 0.0459(13) 0.0328(10) -0.0012(9) 0.0094(9) -0.0111(9)
C14 0.0333(10) 0.0428(13) 0.0342(10) 0.0063(9) 0.0122(9) 0.0018(9)
C15 0.0357(10) 0.0302(10) 0.0314(10) 0.0038(8) 0.0163(8) 0.0020(8)
C16 0.0441(12) 0.0330(12) 0.0422(12) 0.0045(9) 0.0186(10) 0.0100(9)
C17 0.0447(14) 0.0607(18) 0.0423(13) -0.0061(12) 0.0027(11) -0.0108(12)
C18 0.0429(11) 0.0264(10) 0.0387(11) -0.0050(8) 0.0177(9) 0.0004(8)
C19 0.0333(10) 0.0257(9) 0.0295(9) 0.0020(7) 0.0155(8) 0.0000(7)
C20 0.0424(11) 0.0244(10) 0.0314(9) 0.0024(8) 0.0167(9) 0.0019(8)
C21 0.0529(14) 0.0348(12) 0.0493(13) 0.0041(10) 0.0285(11) 0.0079(10)
C22 0.0688(17) 0.0330(13) 0.0556(15) 0.0043(11) 0.0321(14) 0.0171(11)
C23 0.0736(17) 0.0231(11) 0.0479(14) 0.0024(10) 0.0227(13) 0.0019(11)
C24 0.0606(15) 0.0284(12) 0.0454(13) 0.0030(9) 0.0228(12) -0.0076(10)
C25 0.0461(12) 0.0283(11) 0.0392(11) 0.0047(9) 0.0192(10) 0.0000(9)
C26 0.0342(10) 0.0294(10) 0.0262(9) -0.0031(8) 0.0118(8) -0.0036(8)
C27 0.0572(14) 0.0501(15) 0.0359(11) -0.0076(10) 0.0230(11) 0.0068(11)
C28 0.0412(12) 0.0510(15) 0.0367(11) 0.0016(10) 0.0101(10) -0.0147(10)
C29 0.0516(13) 0.0378(12) 0.0294(10) 0.0038(9) 0.0101(9) -0.0043(10)
C30 0.0374(10) 0.0381(11) 0.0245(9) 0.0074(8) 0.0110(8) 0.0060(9)
C31 0.0602(16) 0.0602(18) 0.0371(12) 0.0172(12) 0.0160(11) 0.0253(13)
C32 0.0473(14) 0.088(2) 0.0332(12) 0.0006(12) 0.0191(11) -0.0104(13)
C33 0.0569(14) 0.0496(15) 0.0269(10) 0.0044(10) 0.0082(10) -0.0034(12)
C34 0.0327(10) 0.0277(10) 0.0348(10) 0.0015(8) 0.0180(8) -0.0022(8)
C35 0.0385(11) 0.0478(14) 0.0375(11) 0.0080(10) 0.0181(9) 0.0023(10)
C36 0.0412(12) 0.0390(13) 0.0565(14) 0.0184(11) 0.0262(11) 0.0094(9)
C37 0.0634(16) 0.0352(13) 0.0643(16) 0.0043(11) 0.0437(14) -0.0002(11)
C38 0.0511(14) 0.0498(15) 0.0511(14) -0.0125(12) 0.0296(12) -0.0063(12)
C39 0.0360(11) 0.0460(14) 0.0391(11) -0.0053(10) 0.0164(9) 0.0024(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
As Si 2.3948(6) . ?
As C1 1.9907(19) . ?
As C10 1.9771(19) . ?
Si N1 1.8395(17) . ?
Si N2 1.8328(18) . ?
Si N3 1.570(2) . ?
Si C19 2.290(2) . ?
N1 C19 1.336(2) . ?
N1 C26 1.483(2) . ?
N2 C19 1.344(3) . ?
N2 C30 1.494(2) . ?
N3 C34 1.351(3) . ?
C1 C2 1.399(3) . ?
C1 C6 1.415(3) . ?
C2 C3 1.405(3) . ?
C2 C9 1.509(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.373(3) . ?
C4 C5 1.389(3) . ?
C4 C8 1.510(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(3) . ?
C6 C7 1.511(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.410(3) . ?
C10 C15 1.409(3) . ?
C11 C12 1.391(3) . ?
C11 C18 1.505(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.387(3) . ?
C13 C14 1.391(3) . ?
C13 C17 1.512(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.390(3) . ?
C15 C16 1.513(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
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 C20 1.487(3) . ?
C20 C21 1.388(3) . ?
C20 C25 1.392(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.392(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.374(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.378(4) . ?
C24 H24 0.9500 . ?
C24 C25 1.387(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.527(3) . ?
C26 C28 1.526(3) . ?
C26 C29 1.526(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.521(3) . ?
C30 C32 1.513(3) . ?
C30 C33 1.530(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
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 1.407(3) . ?
C34 C39 1.410(3) . ?
C35 H35 0.9500 . ?
C35 C36 1.403(3) . ?
C36 H36 0.9500 . ?
C36 C37 1.362(4) . ?
C37 H37 0.9500 . ?
C37 C38 1.365(4) . ?
C38 H38 0.9500 . ?
C38 C39 1.384(3) . ?
C39 H39 0.9500 . ?
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 As Si 118.96(6) . . ?
C10 As Si 100.28(6) . . ?
C10 As C1 99.72(8) . . ?
N1 Si As 99.40(6) . . ?
N1 Si C19 35.68(7) . . ?
N2 Si As 98.02(6) . . ?
N2 Si N1 71.63(8) . . ?
N2 Si C19 35.94(7) . . ?
N3 Si As 133.76(8) . . ?
N3 Si N1 117.25(10) . . ?
N3 Si N2 118.91(10) . . ?
N3 Si C19 125.52(9) . . ?
C19 Si As 100.72(5) . . ?
C19 N1 Si 90.89(12) . . ?
C19 N1 C26 130.84(17) . . ?
C26 N1 Si 137.00(13) . . ?
C19 N2 Si 90.91(12) . . ?
C19 N2 C30 129.09(18) . . ?
C30 N2 Si 135.51(14) . . ?
C34 N3 Si 161.25(18) . . ?
C2 C1 As 128.47(15) . . ?
C2 C1 C6 118.78(18) . . ?
C6 C1 As 112.43(15) . . ?
C1 C2 C3 119.32(19) . . ?
C1 C2 C9 124.50(18) . . ?
C3 C2 C9 116.18(19) . . ?
C2 C3 H3 118.7 . . ?
C4 C3 C2 122.7(2) . . ?
C4 C3 H3 118.7 . . ?
C3 C4 C5 117.2(2) . . ?
C3 C4 C8 122.9(2) . . ?
C5 C4 C8 119.9(2) . . ?
C4 C5 H5 118.7 . . ?
C4 C5 C6 122.7(2) . . ?
C6 C5 H5 118.7 . . ?
C1 C6 C7 123.33(18) . . ?
C5 C6 C1 119.24(19) . . ?
C5 C6 C7 117.42(18) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 As 123.16(15) . . ?
C15 C10 As 117.29(15) . . ?
C15 C10 C11 119.54(18) . . ?
C10 C11 C18 123.11(18) . . ?
C12 C11 C10 118.80(19) . . ?
C12 C11 C18 118.09(19) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 C11 122.5(2) . . ?
C13 C12 H12 118.8 . . ?
C12 C13 C14 117.9(2) . . ?
C12 C13 C17 120.7(2) . . ?
C14 C13 C17 121.4(2) . . ?
C13 C14 H14 119.0 . . ?
C15 C14 C13 122.0(2) . . ?
C15 C14 H14 119.0 . . ?
C10 C15 C16 123.00(19) . . ?
C14 C15 C10 119.3(2) . . ?
C14 C15 C16 117.72(19) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C11 C18 H18A 109.5 . . ?
C11 C18 H18B 109.5 . . ?
C11 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 Si 53.43(10) . . ?
N1 C19 N2 106.58(17) . . ?
N1 C19 C20 126.78(18) . . ?
N2 C19 Si 53.15(10) . . ?
N2 C19 C20 126.62(18) . . ?
C20 C19 Si 178.86(15) . . ?
C21 C20 C19 121.3(2) . . ?
C21 C20 C25 120.0(2) . . ?
C25 C20 C19 118.67(19) . . ?
C20 C21 H21 120.3 . . ?
C20 C21 C22 119.4(2) . . ?
C22 C21 H21 120.3 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.6(2) . . ?
C23 C22 H22 119.7 . . ?
C22 C23 H23 120.0 . . ?
C22 C23 C24 119.9(2) . . ?
C24 C23 H23 120.0 . . ?
C23 C24 H24 119.8 . . ?
C23 C24 C25 120.4(2) . . ?
C25 C24 H24 119.8 . . ?
C20 C25 H25 120.2 . . ?
C24 C25 C20 119.6(2) . . ?
C24 C25 H25 120.2 . . ?
N1 C26 C27 111.79(17) . . ?
N1 C26 C28 109.99(17) . . ?
N1 C26 C29 105.77(16) . . ?
C28 C26 C27 111.5(2) . . ?
C28 C26 C29 108.21(19) . . ?
C29 C26 C27 109.39(19) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N2 C30 C31 111.42(18) . . ?
N2 C30 C32 110.20(18) . . ?
N2 C30 C33 106.71(17) . . ?
C31 C30 C33 107.9(2) . . ?
C32 C30 C31 111.3(2) . . ?
C32 C30 C33 109.1(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N3 C34 C35 122.9(2) . . ?
N3 C34 C39 121.6(2) . . ?
C35 C34 C39 115.5(2) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 C34 121.0(2) . . ?
C36 C35 H35 119.5 . . ?
C35 C36 H36 119.3 . . ?
C37 C36 C35 121.4(2) . . ?
C37 C36 H36 119.3 . . ?
C36 C37 H37 120.5 . . ?
C36 C37 C38 119.0(2) . . ?
C38 C37 H37 120.5 . . ?
C37 C38 H38 119.5 . . ?
C37 C38 C39 120.9(2) . . ?
C39 C38 H38 119.5 . . ?
C34 C39 H39 118.9 . . ?
C38 C39 C34 122.2(2) . . ?
C38 C39 H39 118.9 . . ?
_shelx_res_file
;
TITL XCD310 in P2(1)/c
xcd310.res
created by SHELXL-2018/3 at 17:11:17 on 11-Mar-2019
CELL 0.71073 16.8814 12.7921 18.4683 90 116.297 90
ZERR 4 0.0004 0.0003 0.0005 0 0.002 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H As N Si
UNIT 156 200 4 12 4
L.S. 10 0 0
PLAN 10
SIZE 0.213 0.324 0.393
TEMP -123.15
BOND $H
list 4
fmap 2 52
acta 52
REM
REM
REM
WGHT 0.081900 0.151400
FVAR 0.28205
AS 3 0.682475 0.644981 0.342310 11.00000 0.03142 0.02188 =
0.02747 -0.00148 0.01133 -0.00186
SI 5 0.797852 0.675206 0.302800 11.00000 0.03298 0.02231 =
0.02491 0.00066 0.01079 -0.00043
N1 4 0.850627 0.789537 0.366356 11.00000 0.03296 0.02248 =
0.02683 0.00009 0.01188 -0.00230
N2 4 0.752383 0.793519 0.242614 11.00000 0.03803 0.02586 =
0.02597 0.00377 0.01124 0.00230
N3 4 0.858135 0.601446 0.280567 11.00000 0.05662 0.03200 =
0.04869 0.00084 0.03093 0.00343
C1 1 0.688797 0.518868 0.407813 11.00000 0.03678 0.02247 =
0.02478 -0.00133 0.01243 -0.00362
C2 1 0.758972 0.448833 0.444851 11.00000 0.03758 0.02731 =
0.02984 -0.00168 0.01289 -0.00195
C3 1 0.754327 0.372311 0.497413 11.00000 0.04708 0.02971 =
0.03266 0.00280 0.01576 0.00464
AFIX 43
H3 2 0.802671 0.325692 0.522807 11.00000 -1.20000
AFIX 0
C4 1 0.682740 0.362174 0.513568 11.00000 0.05271 0.03021 =
0.02937 0.00051 0.01885 -0.00274
C5 1 0.612191 0.429677 0.473792 11.00000 0.04373 0.03422 =
0.02795 -0.00315 0.01786 -0.00595
AFIX 43
H5 2 0.560533 0.421320 0.481517 11.00000 -1.20000
AFIX 0
C6 1 0.614099 0.508956 0.423146 11.00000 0.03690 0.02874 =
0.02626 -0.00307 0.01462 -0.00321
C7 1 0.535739 0.582049 0.388386 11.00000 0.03834 0.04224 =
0.03535 0.00445 0.01946 0.00118
AFIX 137
H7A 2 0.556564 0.654588 0.397020 11.00000 -1.50000
H7B 2 0.497824 0.570072 0.415241 11.00000 -1.50000
H7C 2 0.502015 0.568886 0.330357 11.00000 -1.50000
AFIX 0
C8 1 0.678694 0.282402 0.572077 11.00000 0.07329 0.04103 =
0.04640 0.01223 0.03255 0.00139
AFIX 137
H8A 2 0.729927 0.235794 0.589520 11.00000 -1.50000
H8B 2 0.624300 0.241355 0.545513 11.00000 -1.50000
H8C 2 0.679228 0.318271 0.619179 11.00000 -1.50000
AFIX 0
C9 1 0.841394 0.448350 0.432264 11.00000 0.04109 0.02990 =
0.04223 0.00596 0.01838 0.00412
AFIX 137
H9A 2 0.831306 0.489925 0.384382 11.00000 -1.50000
H9B 2 0.855894 0.376320 0.424519 11.00000 -1.50000
H9C 2 0.890516 0.478492 0.479716 11.00000 -1.50000
AFIX 0
C10 1 0.585624 0.602279 0.237622 11.00000 0.03080 0.02675 =
0.02598 0.00137 0.01181 -0.00248
C11 1 0.585449 0.506862 0.199281 11.00000 0.03526 0.02681 =
0.03081 0.00019 0.01598 -0.00301
C12 1 0.511321 0.480474 0.128635 11.00000 0.04398 0.03182 =
0.03266 -0.00340 0.01607 -0.00743
AFIX 43
H12 2 0.510885 0.415705 0.103294 11.00000 -1.20000
AFIX 0
C13 1 0.438057 0.545122 0.093813 11.00000 0.03493 0.04585 =
0.03284 -0.00123 0.00940 -0.01105
C14 1 0.440752 0.640616 0.130915 11.00000 0.03325 0.04281 =
0.03418 0.00627 0.01220 0.00177
AFIX 43
H14 2 0.391786 0.686724 0.107095 11.00000 -1.20000
AFIX 0
C15 1 0.512974 0.670564 0.201811 11.00000 0.03572 0.03024 =
0.03138 0.00384 0.01627 0.00199
C16 1 0.508801 0.775587 0.237629 11.00000 0.04407 0.03304 =
0.04216 0.00451 0.01861 0.00999
AFIX 137
H16A 2 0.491919 0.765617 0.281554 11.00000 -1.50000
H16B 2 0.464911 0.819858 0.195734 11.00000 -1.50000
H16C 2 0.566871 0.809317 0.258801 11.00000 -1.50000
AFIX 0
C17 1 0.358313 0.512523 0.017695 11.00000 0.04465 0.06069 =
0.04232 -0.00611 0.00267 -0.01077
AFIX 137
H17A 2 0.374059 0.510188 -0.027375 11.00000 -1.50000
H17B 2 0.310512 0.563110 0.005655 11.00000 -1.50000
H17C 2 0.338676 0.443137 0.025461 11.00000 -1.50000
AFIX 0
C18 1 0.662267 0.432137 0.230692 11.00000 0.04295 0.02641 =
0.03875 -0.00498 0.01773 0.00042
AFIX 137
H18A 2 0.715264 0.468038 0.234511 11.00000 -1.50000
H18B 2 0.649034 0.372618 0.193733 11.00000 -1.50000
H18C 2 0.672521 0.407101 0.284286 11.00000 -1.50000
AFIX 0
C19 1 0.803486 0.854110 0.305554 11.00000 0.03329 0.02572 =
0.02953 0.00197 0.01552 0.00003
C20 1 0.808270 0.970207 0.306487 11.00000 0.04236 0.02443 =
0.03138 0.00243 0.01671 0.00186
C21 1 0.744097 1.030980 0.313840 11.00000 0.05286 0.03480 =
0.04929 0.00406 0.02846 0.00792
AFIX 43
H21 2 0.697050 0.998880 0.320580 11.00000 -1.20000
AFIX 0
C22 1 0.749336 1.139419 0.311243 11.00000 0.06882 0.03303 =
0.05558 0.00432 0.03211 0.01705
AFIX 43
H22 2 0.706160 1.181369 0.317208 11.00000 -1.20000
AFIX 0
C23 1 0.816367 1.186378 0.300132 11.00000 0.07364 0.02311 =
0.04794 0.00241 0.02272 0.00187
AFIX 43
H23 2 0.818825 1.260402 0.297517 11.00000 -1.20000
AFIX 0
C24 1 0.880003 1.125950 0.292791 11.00000 0.06062 0.02840 =
0.04544 0.00297 0.02282 -0.00757
AFIX 43
H24 2 0.926300 1.158571 0.285156 11.00000 -1.20000
AFIX 0
C25 1 0.876909 1.017834 0.296476 11.00000 0.04607 0.02826 =
0.03919 0.00472 0.01919 -0.00004
AFIX 43
H25 2 0.921394 0.976496 0.292191 11.00000 -1.20000
AFIX 0
C26 1 0.906442 0.810619 0.453340 11.00000 0.03422 0.02936 =
0.02620 -0.00315 0.01176 -0.00359
C27 1 0.859291 0.880489 0.489003 11.00000 0.05722 0.05014 =
0.03587 -0.00758 0.02304 0.00681
AFIX 137
H27A 2 0.850582 0.950113 0.464519 11.00000 -1.50000
H27B 2 0.895237 0.886262 0.547515 11.00000 -1.50000
H27C 2 0.801788 0.849945 0.477867 11.00000 -1.50000
AFIX 0
C28 1 0.994584 0.857614 0.465568 11.00000 0.04124 0.05099 =
0.03670 0.00162 0.01010 -0.01467
AFIX 137
H28A 2 1.033172 0.865148 0.523486 11.00000 -1.50000
H28B 2 0.984419 0.926388 0.439608 11.00000 -1.50000
H28C 2 1.022765 0.811484 0.441462 11.00000 -1.50000
AFIX 0
C29 1 0.924518 0.704144 0.494875 11.00000 0.05161 0.03777 =
0.02936 0.00377 0.01013 -0.00434
AFIX 137
H29A 2 0.869187 0.674905 0.491168 11.00000 -1.50000
H29B 2 0.966763 0.712241 0.551806 11.00000 -1.50000
H29C 2 0.949212 0.656915 0.468322 11.00000 -1.50000
AFIX 0
C30 1 0.709165 0.819263 0.154626 11.00000 0.03741 0.03810 =
0.02449 0.00741 0.01097 0.00604
C31 1 0.642095 0.906984 0.135944 11.00000 0.06017 0.06025 =
0.03714 0.01719 0.01605 0.02534
AFIX 137
H31A 2 0.603083 0.891593 0.161134 11.00000 -1.50000
H31B 2 0.606884 0.912853 0.077338 11.00000 -1.50000
H31C 2 0.673110 0.973018 0.157324 11.00000 -1.50000
AFIX 0
C32 1 0.778257 0.846172 0.126426 11.00000 0.04733 0.08831 =
0.03321 0.00058 0.01914 -0.01043
AFIX 137
H32A 2 0.806819 0.912315 0.150993 11.00000 -1.50000
H32B 2 0.750022 0.853123 0.067482 11.00000 -1.50000
H32C 2 0.822689 0.790509 0.142535 11.00000 -1.50000
AFIX 0
C33 1 0.659439 0.721093 0.110428 11.00000 0.05689 0.04957 =
0.02688 0.00439 0.00818 -0.00343
AFIX 137
H33A 2 0.700406 0.661816 0.125295 11.00000 -1.50000
H33B 2 0.634138 0.732542 0.051984 11.00000 -1.50000
H33C 2 0.611923 0.706041 0.125694 11.00000 -1.50000
AFIX 0
C34 1 0.887863 0.516502 0.256630 11.00000 0.03268 0.02775 =
0.03483 0.00151 0.01798 -0.00222
C35 1 0.956727 0.452962 0.310577 11.00000 0.03853 0.04776 =
0.03751 0.00798 0.01814 0.00233
AFIX 43
H35 2 0.984590 0.470008 0.366417 11.00000 -1.20000
AFIX 0
C36 1 0.984877 0.364757 0.283127 11.00000 0.04115 0.03900 =
0.05650 0.01840 0.02617 0.00938
AFIX 43
H36 2 1.030456 0.322071 0.320996 11.00000 -1.20000
AFIX 0
C37 1 0.948210 0.339082 0.203327 11.00000 0.06344 0.03518 =
0.06426 0.00430 0.04370 -0.00021
AFIX 43
H37 2 0.968007 0.279245 0.185555 11.00000 -1.20000
AFIX 0
C38 1 0.882610 0.400578 0.149270 11.00000 0.05110 0.04983 =
0.05106 -0.01248 0.02955 -0.00634
AFIX 43
H38 2 0.857317 0.383793 0.093407 11.00000 -1.20000
AFIX 0
C39 1 0.852409 0.487027 0.174656 11.00000 0.03603 0.04600 =
0.03915 -0.00530 0.01643 0.00245
AFIX 43
H39 2 0.806269 0.527880 0.135583 11.00000 -1.20000
AFIX 0
HKLF 4
REM XCD310 in P2(1)/c
REM wR2 = 0.1222, GooF = S = 1.014, Restrained GooF = 1.014 for all data
REM R1 = 0.0432 for 7412 Fo > 4sig(Fo) and 0.0612 for all 9644 data
REM 409 parameters refined using 0 restraints
END
WGHT 0.0819 0.1514
REM Highest difference peak 0.906, deepest hole -0.433, 1-sigma level 0.075
Q1 1 0.6313 0.6432 0.3006 11.00000 0.05 0.91
Q2 1 0.7199 0.6036 0.3449 11.00000 0.05 0.76
Q3 1 0.7309 0.6689 0.3851 11.00000 0.05 0.71
Q4 1 1.0192 0.4199 0.3220 11.00000 0.05 0.70
Q5 1 0.6397 0.6981 0.3180 11.00000 0.05 0.61
Q6 1 0.9077 0.3726 0.1982 11.00000 0.05 0.49
Q7 1 0.6737 0.7278 0.3424 11.00000 0.05 0.48
Q8 1 0.6774 0.5535 0.3429 11.00000 0.05 0.47
Q9 1 0.5565 0.6419 0.2206 11.00000 0.05 0.42
Q10 1 0.9711 0.5190 0.3288 11.00000 0.05 0.41
;
_shelx_res_checksum 12383
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_xcd150
_database_code_depnum_ccdc_archive 'CCDC 1922576'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record
;
2019-06-12 deposited with the CCDC. 2019-07-05 downloaded from the CCDC.
;
_audit_creation_date 2019-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
#==============================================================================
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C48 H54 As2 Ge N2'
_chemical_formula_sum 'C48 H54 As2 Ge N2'
_chemical_formula_weight 881.36
_chemical_melting_point ?
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'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
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'
_cell_length_a 13.0143(7)
_cell_length_b 18.0257(7)
_cell_length_c 19.1618(10)
_cell_angle_alpha 90
_cell_angle_beta 107.787(4)
_cell_angle_gamma 90
_cell_volume 4280.3(4)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 12144
_cell_measurement_temperature 210
_cell_measurement_theta_max 29.32
_cell_measurement_theta_min 1.99
_shelx_estimated_absorpt_T_max 0.851
_shelx_estimated_absorpt_T_min 0.653
_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_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.368
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_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
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_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_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, \w 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_source 'sealed tube, 12x0.4mm long-fine focus'
_diffrn_source_current 40mA
_diffrn_source_power 2kW
_diffrn_source_voltage 50kV
_diffrn_special_details ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4535
_reflns_number_total 5950
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_data_collection 'STOE X-AREA'
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_structure_solution 'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)'
_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)
;
_refine_diff_density_max 0.953
_refine_diff_density_min -0.737
_refine_diff_density_rms 0.079
_refine_ls_extinction_coef .
_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_R_factor_all 0.0629
_refine_ls_R_factor_gt 0.0425
_refine_ls_restrained_S_all 0.996
_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/[\s^2^(Fo^2^)+(0.0621P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0986
_refine_ls_wR_factor_ref 0.1053
_refine_special_details ?
_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)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
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_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As 0.03156(12) 0.03575(14) 0.03300(15) -0.00054(11) 0.01230(9) -0.00081(9)
Ge 0.0432(2) 0.02923(19) 0.0448(3) 0.000 0.02346(17) 0.000
N 0.0321(10) 0.0325(11) 0.0361(12) 0.0019(9) 0.0141(8) 0.0021(7)
C1 0.0313(11) 0.0456(15) 0.0313(14) 0.0008(11) 0.0110(9) 0.0039(10)
C2 0.0347(12) 0.0472(15) 0.0404(15) 0.0027(12) 0.0153(10) 0.0063(10)
C3 0.0463(15) 0.062(2) 0.0432(18) 0.0132(15) 0.0188(13) 0.0104(13)
C4 0.0421(14) 0.084(3) 0.0339(16) 0.0046(16) 0.0134(12) 0.0164(15)
C5 0.0371(13) 0.077(2) 0.0359(16) -0.0094(15) 0.0057(11) 0.0064(14)
C6 0.0319(11) 0.0563(18) 0.0413(16) -0.0056(13) 0.0101(10) 0.0026(11)
C7 0.0428(14) 0.062(2) 0.055(2) -0.0113(17) 0.0052(13) -0.0111(14)
C8 0.072(2) 0.120(4) 0.037(2) 0.013(2) 0.0140(17) 0.026(2)
C9 0.0545(16) 0.0378(15) 0.0515(19) 0.0036(13) 0.0193(14) 0.0032(12)
C10 0.0385(12) 0.0369(13) 0.0301(13) 0.0003(11) 0.0125(10) 0.0030(10)
C11 0.0413(13) 0.0429(15) 0.0345(15) -0.0007(12) 0.0078(11) 0.0062(11)
C12 0.0504(15) 0.0505(17) 0.0402(17) -0.0080(14) 0.0041(12) 0.0052(13)
C13 0.0635(18) 0.0477(17) 0.0355(16) -0.0051(14) 0.0110(13) 0.0150(14)
C14 0.0540(15) 0.0475(16) 0.0414(17) 0.0018(14) 0.0200(13) 0.0150(13)
C15 0.0415(13) 0.0408(14) 0.0360(15) 0.0051(12) 0.0148(11) 0.0078(10)
C16 0.0422(14) 0.0527(18) 0.057(2) -0.0004(15) 0.0245(13) 0.0036(12)
C17 0.087(3) 0.074(3) 0.060(3) -0.025(2) 0.016(2) 0.016(2)
C18 0.0350(13) 0.063(2) 0.0507(19) -0.0155(16) 0.0064(12) -0.0018(12)
C19 0.0337(11) 0.0370(13) 0.0292(13) 0.0025(10) 0.0103(9) 0.0035(9)
C20 0.0394(13) 0.0395(15) 0.0472(17) 0.0059(12) 0.0143(11) 0.0017(10)
C21 0.0603(17) 0.0381(16) 0.064(2) 0.0123(15) 0.0252(16) 0.0036(13)
C22 0.0614(18) 0.0512(19) 0.061(2) 0.0192(16) 0.0245(16) 0.0208(15)
C23 0.0402(14) 0.067(2) 0.0437(18) 0.0063(15) 0.0088(12) 0.0145(13)
C24 0.0369(12) 0.0478(16) 0.0365(15) 0.0006(12) 0.0112(11) 0.0015(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
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_
_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
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) . . ?
_shelx_res_file
;
TITL 5-XCD150 in C2/c
xcd150.res
created by SHELXL-2018/3 at 12:52:01 on 07-Mar-2019
CELL 0.71073 13.0143 18.0257 19.1618 90 107.787 90
ZERR 4 0.0007 0.0007 0.001 0 0.004 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H As Ge N
UNIT 192 216 8 4 8
L.S. 10
PLAN 10
SIZE 0.073 0.151 0.204
TEMP 210
BOND
list 4
fmap 2 53
acta 52
REM
REM
REM
WGHT 0.062100
FVAR 0.20500
AS 3 0.339291 0.735809 0.344496 11.00000 0.03156 0.03575 =
0.03300 -0.00054 0.01230 -0.00081
GE 4 0.500000 0.786267 0.250000 10.50000 0.04315 0.02923 =
0.04480 0.00000 0.02346 0.00000
N 5 0.461450 0.720165 0.313581 11.00000 0.03209 0.03245 =
0.03611 0.00186 0.01414 0.00209
C1 1 0.255081 0.793651 0.257240 11.00000 0.03131 0.04561 =
0.03133 0.00080 0.01096 0.00386
C2 1 0.271631 0.868219 0.240502 11.00000 0.03474 0.04723 =
0.04036 0.00273 0.01534 0.00625
C3 1 0.215820 0.894951 0.171005 11.00000 0.04628 0.06161 =
0.04324 0.01317 0.01880 0.01042
AFIX 43
H3 2 0.227969 0.943617 0.159457 11.00000 -1.20000
AFIX 0
C4 1 0.142833 0.852267 0.118135 11.00000 0.04214 0.08412 =
0.03390 0.00461 0.01343 0.01640
C5 1 0.122638 0.781076 0.137085 11.00000 0.03708 0.07666 =
0.03595 -0.00940 0.00571 0.00638
AFIX 43
H5 2 0.072092 0.752190 0.103176 11.00000 -1.20000
AFIX 0
C6 1 0.176189 0.751372 0.205867 11.00000 0.03191 0.05631 =
0.04135 -0.00565 0.01008 0.00257
C7 1 0.145925 0.673484 0.221730 11.00000 0.04281 0.06218 =
0.05479 -0.01127 0.00519 -0.01111
AFIX 137
H7A 2 0.205694 0.640738 0.225947 11.00000 -1.50000
H7B 2 0.084722 0.657055 0.182490 11.00000 -1.50000
H7C 2 0.128169 0.673268 0.266812 11.00000 -1.50000
AFIX 0
C8 1 0.086622 0.883766 0.042506 11.00000 0.07209 0.12043 =
0.03746 0.01344 0.01397 0.02552
AFIX 137
H8A 2 0.051816 0.929588 0.047337 11.00000 -1.50000
H8B 2 0.033693 0.849006 0.015123 11.00000 -1.50000
H8C 2 0.138854 0.892600 0.017289 11.00000 -1.50000
AFIX 0
C9 1 0.345039 0.922173 0.292867 11.00000 0.05446 0.03782 =
0.05150 0.00356 0.01929 0.00321
AFIX 137
H9A 2 0.310606 0.939296 0.327611 11.00000 -1.50000
H9B 2 0.359626 0.963659 0.265928 11.00000 -1.50000
H9C 2 0.411559 0.897869 0.318356 11.00000 -1.50000
AFIX 0
C10 1 0.372740 0.811097 0.423392 11.00000 0.03845 0.03692 =
0.03014 0.00032 0.01245 0.00302
C11 1 0.473974 0.840095 0.464408 11.00000 0.04128 0.04288 =
0.03452 -0.00069 0.00775 0.00621
C12 1 0.478717 0.890475 0.519893 11.00000 0.05040 0.05048 =
0.04023 -0.00803 0.00413 0.00516
AFIX 43
H12 2 0.545454 0.910522 0.545451 11.00000 -1.20000
AFIX 0
C13 1 0.389142 0.912525 0.539257 11.00000 0.06348 0.04769 =
0.03554 -0.00510 0.01099 0.01495
C14 1 0.290506 0.881646 0.500488 11.00000 0.05404 0.04752 =
0.04142 0.00179 0.02003 0.01502
AFIX 43
H14 2 0.229404 0.894526 0.513252 11.00000 -1.20000
AFIX 0
C15 1 0.280212 0.832109 0.443224 11.00000 0.04146 0.04078 =
0.03596 0.00506 0.01481 0.00781
C16 1 0.168802 0.802143 0.403755 11.00000 0.04219 0.05270 =
0.05685 -0.00037 0.02446 0.00360
AFIX 137
H16A 2 0.145428 0.820809 0.354485 11.00000 -1.50000
H16B 2 0.119129 0.817700 0.429000 11.00000 -1.50000
H16C 2 0.171264 0.748936 0.402774 11.00000 -1.50000
AFIX 0
C17 1 0.398175 0.967310 0.600313 11.00000 0.08677 0.07376 =
0.06017 -0.02504 0.01633 0.01615
AFIX 137
H17A 2 0.348501 1.007400 0.582542 11.00000 -1.50000
H17B 2 0.470414 0.986435 0.617227 11.00000 -1.50000
H17C 2 0.381360 0.942973 0.640040 11.00000 -1.50000
AFIX 0
C18 1 0.578726 0.819490 0.450366 11.00000 0.03504 0.06336 =
0.05068 -0.01552 0.00642 -0.00179
AFIX 137
H18A 2 0.583099 0.766538 0.446729 11.00000 -1.50000
H18B 2 0.638450 0.837028 0.490069 11.00000 -1.50000
H18C 2 0.581038 0.841843 0.405397 11.00000 -1.50000
AFIX 0
C19 1 0.513701 0.650458 0.333427 11.00000 0.03374 0.03699 =
0.02920 0.00245 0.01035 0.00351
C20 1 0.457851 0.583490 0.327038 11.00000 0.03943 0.03949 =
0.04722 0.00588 0.01428 0.00170
AFIX 43
H20 2 0.382805 0.583760 0.311568 11.00000 -1.20000
AFIX 0
C21 1 0.512287 0.516645 0.343345 11.00000 0.06030 0.03811 =
0.06387 0.01231 0.02523 0.00357
AFIX 43
H21 2 0.473596 0.472593 0.338814 11.00000 -1.20000
AFIX 0
C22 1 0.623846 0.514972 0.366330 11.00000 0.06139 0.05119 =
0.06104 0.01919 0.02452 0.02080
AFIX 43
H22 2 0.660267 0.469969 0.376812 11.00000 -1.20000
AFIX 0
C23 1 0.680750 0.580688 0.373595 11.00000 0.04019 0.06702 =
0.04372 0.00630 0.00883 0.01454
AFIX 43
H23 2 0.755786 0.579814 0.389191 11.00000 -1.20000
AFIX 0
C24 1 0.626845 0.648041 0.357806 11.00000 0.03685 0.04777 =
0.03649 0.00064 0.01120 0.00154
AFIX 43
H24 2 0.666092 0.691936 0.363441 11.00000 -1.20000
AFIX 0
HKLF 4
REM 5-XCD150 in C2/c
REM wR2 = 0.1053, GooF = S = 0.996, Restrained GooF = 0.996 for all data
REM R1 = 0.0425 for 4535 Fo > 4sig(Fo) and 0.0629 for all 5950 data
REM 246 parameters refined using 0 restraints
END
WGHT 0.0621 0.0000
REM Highest difference peak 0.953, deepest hole -0.737, 1-sigma level 0.079
Q1 1 0.2699 0.7383 0.3411 11.00000 0.05 0.95
Q2 1 0.4073 0.7366 0.3450 11.00000 0.05 0.84
Q3 1 0.4236 0.7843 0.2449 11.00000 0.05 0.75
Q4 1 0.3078 0.6993 0.3598 11.00000 0.05 0.65
Q5 1 0.3797 0.7390 0.4000 11.00000 0.05 0.62
Q6 1 0.2801 0.7422 0.2824 11.00000 0.05 0.58
Q7 1 0.3647 0.6967 0.3204 11.00000 0.05 0.55
Q8 1 0.5354 0.7827 0.3039 11.00000 0.05 0.54
Q9 1 0.4616 0.7453 0.2656 11.00000 0.05 0.53
Q10 1 0.3395 0.7796 0.3219 11.00000 0.05 0.51
;
_shelx_res_checksum 87095
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_xcd430
_database_code_depnum_ccdc_archive 'CCDC 1922574'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record
;
2019-06-12 deposited with the CCDC. 2019-07-05 downloaded from the CCDC.
;
_audit_creation_date 2019-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
#==============================================================================
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C39 H50 As Ge N3'
_chemical_formula_sum 'C39 H50 As Ge N3'
_chemical_formula_weight 708.33
_chemical_melting_point ?
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'
_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.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.1929(5)
_cell_length_b 12.0657(7)
_cell_length_c 16.2153(9)
_cell_angle_alpha 91.416(5)
_cell_angle_beta 91.029(4)
_cell_angle_gamma 93.834(4)
_cell_volume 1793.66(17)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 11760
_cell_measurement_temperature 150
_cell_measurement_theta_max 29.53
_cell_measurement_theta_min 2.08
_shelx_estimated_absorpt_T_max 0.643
_shelx_estimated_absorpt_T_min 0.479
_exptl_absorpt_coefficient_mu 1.800
_exptl_absorpt_correction_T_max 0.3817
_exptl_absorpt_correction_T_min 0.3110
_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.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.312
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description prism
_exptl_crystal_F_000 740
_exptl_crystal_size_max 0.48
_exptl_crystal_size_mid 0.378
_exptl_crystal_size_min 0.269
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0293
_diffrn_reflns_av_unetI/netI 0.0720
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 16
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 18292
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 29.191
_diffrn_reflns_theta_min 1.692
_diffrn_ambient_temperature 150
_diffrn_detector 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type 'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
197 frames, detector distance = 100 mm
;
_diffrn_measurement_device '2-circle diffractometer'
_diffrn_measurement_device_type 'STOE IPDS II'
_diffrn_measurement_method 'rotation method, \w 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_source 'sealed tube, 12x0.4mm long-fine focus'
_diffrn_source_current 40mA
_diffrn_source_power 2kW
_diffrn_source_target ?
_diffrn_source_type ?
_diffrn_source_voltage 50kV
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 6232
_reflns_number_total 9516
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_data_collection 'STOE X-AREA'
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_structure_solution 'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)'
_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)
;
_refine_diff_density_max 0.399
_refine_diff_density_min -0.425
_refine_diff_density_rms 0.058
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.879
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 409
_refine_ls_number_reflns 9516
_refine_ls_number_restraints 12
_refine_ls_R_factor_all 0.0541
_refine_ls_R_factor_gt 0.0278
_refine_ls_restrained_S_all 0.880
_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/[\s^2^(Fo^2^)+(0.0268P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0555
_refine_ls_wR_factor_ref 0.0577
_refine_special_details ?
_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. Uiso/Uaniso restraints and constraints
N1 \\sim C19 \\sim N2: within 2A with sigma of 0.002 and sigma for terminal
atoms of 0.004
3.a Aromatic/amide H refined with riding coordinates:
C3(H3), C5(H5), C12(H12), C14(H14), C21(H21), C22(H22), C23(H23), C24(H24),
C25(H25), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
3.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), C27(H27A,H27B,H27C), C28(H28A,H28B,
H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
H33B,H33C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
As As 0.45250(2) 0.86501(2) 0.35397(2) 0.02007(5) Uani 1 1 d . . . . .
Ge Ge 0.46859(2) 0.66583(2) 0.21249(2) 0.02197(6) Uani 1 1 d . . . . .
N1 N 0.45108(15) 0.49485(12) 0.22077(9) 0.0220(3) Uani 1 1 d . U . . .
N2 N 0.28429(15) 0.58920(12) 0.16630(9) 0.0208(3) Uani 1 1 d . U . . .
N3 N 0.39520(15) 0.72042(12) 0.31435(9) 0.0198(3) Uani 1 1 d . . . . .
C1 C 0.55016(18) 0.92370(14) 0.25505(11) 0.0207(4) Uani 1 1 d . . . . .
C2 C 0.69296(19) 0.90641(15) 0.22919(11) 0.0230(4) Uani 1 1 d . . . . .
C3 C 0.7454(2) 0.95983(16) 0.16001(12) 0.0282(4) Uani 1 1 d . . . . .
H3 H 0.842103 0.948778 0.143488 0.034 Uiso 1 1 calc R . . . .
C4 C 0.6629(2) 1.02863(16) 0.11394(12) 0.0326(5) Uani 1 1 d . . . . .
C5 C 0.5221(2) 1.04372(16) 0.13973(12) 0.0314(5) Uani 1 1 d . . . . .
H5 H 0.463086 1.090024 0.108817 0.038 Uiso 1 1 calc R . . . .
C6 C 0.46519(19) 0.99363(15) 0.20879(12) 0.0257(4) Uani 1 1 d . . . . .
C7 C 0.3129(2) 1.01945(17) 0.23380(13) 0.0339(5) Uani 1 1 d . . . . .
H7A H 0.252673 0.949921 0.239037 0.051 Uiso 1 1 calc GR . . . .
H7B H 0.269646 1.064751 0.191702 0.051 Uiso 1 1 calc GR . . . .
H7C H 0.317759 1.060388 0.286843 0.051 Uiso 1 1 calc GR . . . .
C8 C 0.7214(3) 1.08573(19) 0.03875(14) 0.0463(6) Uani 1 1 d . . . . .
H8A H 0.727836 1.166351 0.048804 0.069 Uiso 1 1 calc GR . . . .
H8B H 0.655924 1.066860 -0.008601 0.069 Uiso 1 1 calc GR . . . .
H8C H 0.818600 1.061156 0.027108 0.069 Uiso 1 1 calc GR . . . .
C9 C 0.79108(19) 0.83166(16) 0.27362(12) 0.0294(5) Uani 1 1 d . . . . .
H9A H 0.842163 0.873343 0.319329 0.044 Uiso 1 1 calc GR . . . .
H9B H 0.862485 0.804501 0.235169 0.044 Uiso 1 1 calc GR . . . .
H9C H 0.732489 0.768450 0.295292 0.044 Uiso 1 1 calc GR . . . .
C10 C 0.61465(18) 0.85748(15) 0.43557(11) 0.0216(4) Uani 1 1 d . . . . .
C11 C 0.63880(19) 0.76455(15) 0.48411(11) 0.0236(4) Uani 1 1 d . . . . .
C12 C 0.74695(19) 0.77514(17) 0.54562(12) 0.0279(4) Uani 1 1 d . . . . .
H12 H 0.763510 0.712557 0.578075 0.034 Uiso 1 1 calc R . . . .
C13 C 0.83111(19) 0.87274(18) 0.56144(12) 0.0292(5) Uani 1 1 d . . . . .
C14 C 0.79943(19) 0.96451(17) 0.51689(12) 0.0289(4) Uani 1 1 d . . . . .
H14 H 0.853220 1.033292 0.528453 0.035 Uiso 1 1 calc R . . . .
C15 C 0.69088(19) 0.95929(15) 0.45546(11) 0.0240(4) Uani 1 1 d . . . . .
C16 C 0.6578(2) 1.06606(15) 0.41421(12) 0.0301(5) Uani 1 1 d . . . . .
H16A H 0.702077 1.129506 0.446724 0.045 Uiso 1 1 calc GR . . . .
H16B H 0.551989 1.071366 0.410548 0.045 Uiso 1 1 calc GR . . . .
H16C H 0.697930 1.066481 0.358623 0.045 Uiso 1 1 calc GR . . . .
C17 C 0.9520(2) 0.8777(2) 0.62628(14) 0.0437(6) Uani 1 1 d . . . . .
H17A H 0.914974 0.844663 0.677051 0.066 Uiso 1 1 calc GR . . . .
H17B H 0.986225 0.955326 0.637614 0.066 Uiso 1 1 calc GR . . . .
H17C H 1.032934 0.836300 0.606163 0.066 Uiso 1 1 calc GR . . . .
C18 C 0.5494(2) 0.65593(16) 0.47563(13) 0.0336(5) Uani 1 1 d . . . . .
H18A H 0.590287 0.601757 0.512013 0.050 Uiso 1 1 calc GR . . . .
H18B H 0.551002 0.628331 0.418323 0.050 Uiso 1 1 calc GR . . . .
H18C H 0.448671 0.666822 0.491012 0.050 Uiso 1 1 calc GR . . . .
C19 C 0.33327(19) 0.48832(15) 0.17122(11) 0.0216(4) Uani 1 1 d . U . . .
C20 C 0.26734(19) 0.38617(15) 0.12727(12) 0.0259(4) Uani 1 1 d . . . . .
C21 C 0.1592(2) 0.32027(16) 0.16561(13) 0.0324(5) Uani 1 1 d . . . . .
H21 H 0.128431 0.339961 0.219321 0.039 Uiso 1 1 calc R . . . .
C22 C 0.0968(2) 0.22587(17) 0.12485(16) 0.0427(6) Uani 1 1 d . . . . .
H22 H 0.022604 0.180937 0.150400 0.051 Uiso 1 1 calc R . . . .
C23 C 0.1430(3) 0.19731(18) 0.04677(17) 0.0488(7) Uani 1 1 d . . . . .
H23 H 0.100706 0.132401 0.019039 0.059 Uiso 1 1 calc R . . . .
C24 C 0.2492(3) 0.26191(19) 0.00932(15) 0.0443(6) Uani 1 1 d . . . . .
H24 H 0.280421 0.241793 -0.044212 0.053 Uiso 1 1 calc R . . . .
C25 C 0.3107(2) 0.35603(17) 0.04922(13) 0.0342(5) Uani 1 1 d . . . . .
H25 H 0.383949 0.400832 0.022767 0.041 Uiso 1 1 calc R . . . .
C26 C 0.56082(19) 0.41160(16) 0.23350(12) 0.0261(4) Uani 1 1 d . . . . .
C27 C 0.6423(2) 0.38914(19) 0.15474(13) 0.0403(6) Uani 1 1 d . . . . .
H27A H 0.576134 0.348936 0.114556 0.060 Uiso 1 1 calc GR . . . .
H27B H 0.724507 0.344184 0.167111 0.060 Uiso 1 1 calc GR . . . .
H27C H 0.678774 0.459811 0.131757 0.060 Uiso 1 1 calc GR . . . .
C28 C 0.4915(2) 0.30401(17) 0.26601(14) 0.0399(5) Uani 1 1 d . . . . .
H28A H 0.433322 0.320393 0.314340 0.060 Uiso 1 1 calc GR . . . .
H28B H 0.567987 0.255356 0.281718 0.060 Uiso 1 1 calc GR . . . .
H28C H 0.428335 0.266826 0.222973 0.060 Uiso 1 1 calc GR . . . .
C29 C 0.6685(2) 0.46397(18) 0.29813(14) 0.0399(6) Uani 1 1 d . . . . .
H29A H 0.709735 0.535417 0.278696 0.060 Uiso 1 1 calc GR . . . .
H29B H 0.747021 0.414346 0.307285 0.060 Uiso 1 1 calc GR . . . .
H29C H 0.617848 0.475815 0.349964 0.060 Uiso 1 1 calc GR . . . .
C30 C 0.15369(19) 0.62766(15) 0.12315(11) 0.0237(4) Uani 1 1 d . . . . .
C31 C 0.1591(2) 0.60559(17) 0.02988(12) 0.0327(5) Uani 1 1 d . . . . .
H31A H 0.251519 0.637798 0.009001 0.049 Uiso 1 1 calc GR . . . .
H31B H 0.077772 0.639565 0.002614 0.049 Uiso 1 1 calc GR . . . .
H31C H 0.151420 0.525276 0.018347 0.049 Uiso 1 1 calc GR . . . .
C32 C 0.1591(2) 0.75251(15) 0.14018(12) 0.0286(4) Uani 1 1 d . . . . .
H32A H 0.150858 0.767118 0.199577 0.043 Uiso 1 1 calc GR . . . .
H32B H 0.078096 0.784026 0.110767 0.043 Uiso 1 1 calc GR . . . .
H32C H 0.251754 0.786767 0.121164 0.043 Uiso 1 1 calc GR . . . .
C33 C 0.01349(19) 0.57488(16) 0.15866(13) 0.0307(5) Uani 1 1 d . . . . .
H33A H 0.005861 0.495027 0.145274 0.046 Uiso 1 1 calc GR . . . .
H33B H -0.070622 0.609291 0.134766 0.046 Uiso 1 1 calc GR . . . .
H33C H 0.015268 0.586461 0.218708 0.046 Uiso 1 1 calc GR . . . .
C34 C 0.26198(18) 0.67674(15) 0.34841(11) 0.0204(4) Uani 1 1 d . . . . .
C35 C 0.14898(18) 0.74326(16) 0.36841(11) 0.0244(4) Uani 1 1 d . . . . .
H35 H 0.160440 0.820861 0.359544 0.029 Uiso 1 1 calc R . . . .
C36 C 0.02016(19) 0.69873(17) 0.40096(12) 0.0294(5) Uani 1 1 d . . . . .
H36 H -0.053907 0.746437 0.415559 0.035 Uiso 1 1 calc R . . . .
C37 C -0.00166(19) 0.58679(17) 0.41233(12) 0.0302(5) Uani 1 1 d . . . . .
H37 H -0.090990 0.556375 0.433469 0.036 Uiso 1 1 calc R . . . .
C38 C 0.1090(2) 0.51848(17) 0.39244(12) 0.0303(5) Uani 1 1 d . . . . .
H38 H 0.094967 0.440598 0.399498 0.036 Uiso 1 1 calc R . . . .
C39 C 0.24013(19) 0.56324(15) 0.36230(11) 0.0238(4) Uani 1 1 d . . . . .
H39 H 0.316125 0.515788 0.350974 0.029 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As 0.02213(10) 0.01761(10) 0.02063(11) -0.00052(8) 0.00295(8) 0.00236(8)
Ge 0.02349(10) 0.02026(11) 0.02179(12) -0.00235(9) 0.00661(8) -0.00183(8)
N1 0.0234(7) 0.0198(8) 0.0229(8) -0.0024(6) 0.0024(6) 0.0023(6)
N2 0.0247(7) 0.0191(8) 0.0185(8) 0.0009(6) 0.0011(6) 0.0005(6)
N3 0.0226(7) 0.0196(8) 0.0169(8) -0.0008(6) 0.0038(6) -0.0007(6)
C1 0.0269(9) 0.0150(9) 0.0196(10) -0.0003(7) 0.0012(7) -0.0024(7)
C2 0.0267(9) 0.0211(10) 0.0205(10) -0.0035(8) 0.0003(7) -0.0025(8)
C3 0.0306(10) 0.0273(11) 0.0257(12) -0.0034(9) 0.0057(8) -0.0051(8)
C4 0.0517(13) 0.0214(11) 0.0233(12) 0.0003(9) 0.0033(9) -0.0098(9)
C5 0.0466(12) 0.0214(11) 0.0260(12) 0.0048(9) -0.0073(9) 0.0012(9)
C6 0.0329(10) 0.0168(10) 0.0269(11) 0.0003(8) -0.0050(8) -0.0003(8)
C7 0.0342(11) 0.0285(11) 0.0401(13) 0.0070(10) -0.0043(9) 0.0099(9)
C8 0.0703(16) 0.0373(14) 0.0308(14) 0.0094(11) 0.0113(11) -0.0062(11)
C9 0.0254(10) 0.0335(12) 0.0304(12) 0.0007(9) 0.0056(8) 0.0072(8)
C10 0.0229(9) 0.0235(10) 0.0183(10) -0.0044(8) 0.0024(7) 0.0025(7)
C11 0.0259(9) 0.0255(10) 0.0198(10) -0.0020(8) 0.0051(7) 0.0047(8)
C12 0.0295(10) 0.0354(12) 0.0199(11) 0.0027(9) 0.0053(8) 0.0079(9)
C13 0.0243(10) 0.0444(13) 0.0188(11) -0.0029(9) 0.0041(8) 0.0023(9)
C14 0.0283(10) 0.0321(12) 0.0251(12) -0.0080(9) 0.0053(8) -0.0055(8)
C15 0.0272(9) 0.0254(10) 0.0195(10) -0.0020(8) 0.0070(8) 0.0014(8)
C16 0.0351(11) 0.0229(11) 0.0314(12) -0.0047(9) 0.0019(9) -0.0024(8)
C17 0.0320(11) 0.0651(17) 0.0332(14) 0.0023(12) -0.0047(9) -0.0014(11)
C18 0.0453(12) 0.0247(11) 0.0306(12) 0.0081(9) -0.0050(9) 0.0010(9)
C19 0.0259(8) 0.0219(8) 0.0166(8) 0.0007(7) 0.0067(7) -0.0018(7)
C20 0.0314(10) 0.0197(10) 0.0263(11) -0.0013(8) -0.0061(8) 0.0009(8)
C21 0.0368(11) 0.0270(11) 0.0329(13) 0.0023(9) -0.0085(9) -0.0003(9)
C22 0.0409(12) 0.0249(12) 0.0609(17) 0.0089(11) -0.0213(11) -0.0044(9)
C23 0.0595(15) 0.0227(12) 0.0633(18) -0.0109(12) -0.0331(13) 0.0105(11)
C24 0.0561(14) 0.0378(14) 0.0396(15) -0.0151(11) -0.0169(11) 0.0188(12)
C25 0.0414(12) 0.0312(12) 0.0301(12) -0.0064(10) -0.0059(9) 0.0080(9)
C26 0.0233(9) 0.0267(11) 0.0289(12) -0.0037(9) 0.0024(8) 0.0064(8)
C27 0.0317(11) 0.0522(15) 0.0381(14) -0.0085(11) 0.0078(9) 0.0126(10)
C28 0.0387(12) 0.0307(12) 0.0518(16) 0.0106(11) 0.0012(10) 0.0101(9)
C29 0.0360(12) 0.0412(13) 0.0432(15) -0.0088(11) -0.0093(10) 0.0146(10)
C30 0.0272(10) 0.0257(10) 0.0183(10) 0.0016(8) -0.0005(7) 0.0014(8)
C31 0.0416(12) 0.0341(12) 0.0228(12) -0.0007(9) -0.0046(9) 0.0081(9)
C32 0.0356(11) 0.0276(11) 0.0230(11) 0.0046(9) -0.0002(8) 0.0049(9)
C33 0.0262(10) 0.0308(11) 0.0353(13) 0.0057(9) 0.0008(8) 0.0021(8)
C34 0.0217(9) 0.0255(10) 0.0139(10) 0.0009(8) 0.0014(7) 0.0002(7)
C35 0.0263(9) 0.0252(10) 0.0220(11) 0.0030(8) 0.0022(8) 0.0017(8)
C36 0.0235(9) 0.0410(13) 0.0243(11) 0.0029(9) 0.0042(8) 0.0059(9)
C37 0.0237(9) 0.0447(13) 0.0221(11) 0.0099(9) 0.0044(8) -0.0031(9)
C38 0.0345(11) 0.0299(11) 0.0263(12) 0.0077(9) 0.0048(8) -0.0030(9)
C39 0.0272(9) 0.0262(11) 0.0182(10) 0.0025(8) 0.0047(7) 0.0016(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
As N3 1.8824(14) . ?
As C1 1.9757(18) . ?
As C10 1.9834(17) . ?
Ge N1 2.0665(15) . ?
Ge N2 1.9993(14) . ?
Ge N3 1.9138(14) . ?
Ge C19 2.4751(19) . ?
N1 C19 1.334(2) . ?
N1 C26 1.486(2) . ?
N2 C19 1.329(2) . ?
N2 C30 1.485(2) . ?
N3 C34 1.427(2) . ?
C1 C2 1.412(2) . ?
C1 C6 1.408(2) . ?
C2 C3 1.386(3) . ?
C2 C9 1.504(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.385(3) . ?
C4 C5 1.389(3) . ?
C4 C8 1.505(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.380(3) . ?
C6 C7 1.515(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.413(2) . ?
C10 C15 1.400(3) . ?
C11 C12 1.393(2) . ?
C11 C18 1.501(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.381(3) . ?
C13 C14 1.381(3) . ?
C13 C17 1.513(3) . ?
C14 H14 0.9500 . ?
C14 C15 1.395(3) . ?
C15 C16 1.512(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
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 C20 1.495(3) . ?
C20 C21 1.396(3) . ?
C20 C25 1.381(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.387(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.386(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.368(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.376(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.520(3) . ?
C26 C28 1.518(3) . ?
C26 C29 1.524(3) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.531(3) . ?
C30 C32 1.522(3) . ?
C30 C33 1.527(2) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
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 1.392(2) . ?
C34 C39 1.395(2) . ?
C35 H35 0.9500 . ?
C35 C36 1.386(2) . ?
C36 H36 0.9500 . ?
C36 C37 1.370(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.389(3) . ?
C38 H38 0.9500 . ?
C38 C39 1.389(2) . ?
C39 H39 0.9500 . ?
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
N3 As C1 99.45(7) . . ?
N3 As C10 109.08(7) . . ?
C1 As C10 103.56(7) . . ?
N1 Ge C19 32.60(5) . . ?
N2 Ge N1 64.13(6) . . ?
N2 Ge C19 32.41(5) . . ?
N3 Ge N1 105.04(6) . . ?
N3 Ge N2 98.70(6) . . ?
N3 Ge C19 109.63(6) . . ?
C19 N1 Ge 90.80(11) . . ?
C19 N1 C26 129.02(15) . . ?
C26 N1 Ge 132.59(11) . . ?
C19 N2 Ge 93.89(11) . . ?
C19 N2 C30 130.69(16) . . ?
C30 N2 Ge 133.99(12) . . ?
As N3 Ge 120.36(8) . . ?
C34 N3 As 113.13(11) . . ?
C34 N3 Ge 122.75(11) . . ?
C2 C1 As 127.47(13) . . ?
C6 C1 As 113.78(13) . . ?
C6 C1 C2 118.70(17) . . ?
C1 C2 C9 122.64(17) . . ?
C3 C2 C1 119.04(17) . . ?
C3 C2 C9 118.32(16) . . ?
C2 C3 H3 118.6 . . ?
C4 C3 C2 122.81(18) . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C5 117.37(19) . . ?
C3 C4 C8 122.12(19) . . ?
C5 C4 C8 120.51(19) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 C4 122.16(18) . . ?
C6 C5 H5 118.9 . . ?
C1 C6 C7 122.04(17) . . ?
C5 C6 C1 119.90(17) . . ?
C5 C6 C7 118.02(17) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 C9 H9A 109.5 . . ?
C2 C9 H9B 109.5 . . ?
C2 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 As 124.80(14) . . ?
C15 C10 As 115.06(13) . . ?
C15 C10 C11 119.02(17) . . ?
C10 C11 C18 123.49(17) . . ?
C12 C11 C10 118.59(18) . . ?
C12 C11 C18 117.86(17) . . ?
C11 C12 H12 118.6 . . ?
C13 C12 C11 122.81(18) . . ?
C13 C12 H12 118.6 . . ?
C12 C13 C14 117.62(17) . . ?
C12 C13 C17 120.43(19) . . ?
C14 C13 C17 121.94(19) . . ?
C13 C14 H14 119.0 . . ?
C13 C14 C15 122.01(18) . . ?
C15 C14 H14 119.0 . . ?
C10 C15 C16 122.52(17) . . ?
C14 C15 C10 119.58(17) . . ?
C14 C15 C16 117.88(17) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C11 C18 H18A 109.5 . . ?
C11 C18 H18B 109.5 . . ?
C11 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 Ge 56.60(9) . . ?
N1 C19 C20 126.47(16) . . ?
N2 C19 Ge 53.70(9) . . ?
N2 C19 N1 108.33(16) . . ?
N2 C19 C20 125.20(16) . . ?
C20 C19 Ge 166.62(13) . . ?
C21 C20 C19 119.39(18) . . ?
C25 C20 C19 121.31(18) . . ?
C25 C20 C21 119.30(19) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 C20 119.6(2) . . ?
C22 C21 H21 120.2 . . ?
C21 C22 H22 120.1 . . ?
C23 C22 C21 119.8(2) . . ?
C23 C22 H22 120.1 . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.5(2) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 120.0 . . ?
C23 C24 C25 120.0(2) . . ?
C25 C24 H24 120.0 . . ?
C20 C25 H25 119.6 . . ?
C24 C25 C20 120.8(2) . . ?
C24 C25 H25 119.6 . . ?
N1 C26 C27 111.37(16) . . ?
N1 C26 C28 111.50(14) . . ?
N1 C26 C29 105.47(15) . . ?
C27 C26 C29 108.81(16) . . ?
C28 C26 C27 110.41(17) . . ?
C28 C26 C29 109.12(18) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N2 C30 C31 111.47(14) . . ?
N2 C30 C32 105.26(14) . . ?
N2 C30 C33 111.09(15) . . ?
C32 C30 C31 109.06(15) . . ?
C32 C30 C33 108.65(15) . . ?
C33 C30 C31 111.08(16) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 N3 122.53(16) . . ?
C35 C34 C39 117.26(16) . . ?
C39 C34 N3 120.21(15) . . ?
C34 C35 H35 119.3 . . ?
C36 C35 C34 121.45(18) . . ?
C36 C35 H35 119.3 . . ?
C35 C36 H36 119.6 . . ?
C37 C36 C35 120.81(18) . . ?
C37 C36 H36 119.6 . . ?
C36 C37 H37 120.6 . . ?
C36 C37 C38 118.88(17) . . ?
C38 C37 H37 120.6 . . ?
C37 C38 H38 119.8 . . ?
C37 C38 C39 120.48(18) . . ?
C39 C38 H38 119.8 . . ?
C34 C39 H39 119.5 . . ?
C38 C39 C34 121.07(17) . . ?
C38 C39 H39 119.5 . . ?
_shelx_res_file
;
TITL 2-XCD430 in P-1
xcd430.res
created by SHELXL-2018/3 at 17:22:46 on 11-Mar-2019
CELL 0.71073 9.1929 12.0657 16.2153 91.416 91.029 93.834
ZERR 2 0.0005 0.0007 0.0009 0.005 0.004 0.004
LATT 1
SFAC C H As Ge N
UNIT 78 100 2 2 6
SIMU 0.002 0.004 2 N1 C19 N2
L.S. 10 0 0
PLAN 10
SIZE 0.269 0.378 0.48
TEMP -123.15
BOND $H
list 4
fmap 2 52
acta 52
OMIT 0 -1 1
OMIT -1 -2 6
OMIT -9 4 4
OMIT -3 2 4
REM
REM
REM
WGHT 0.026800
FVAR 0.51893
AS 3 0.452504 0.865013 0.353974 11.00000 0.02213 0.01761 =
0.02063 -0.00052 0.00295 0.00236
GE 4 0.468593 0.665833 0.212492 11.00000 0.02349 0.02026 =
0.02179 -0.00235 0.00661 -0.00183
N1 5 0.451078 0.494846 0.220774 11.00000 0.02336 0.01978 =
0.02290 -0.00241 0.00242 0.00228
N2 5 0.284287 0.589199 0.166298 11.00000 0.02470 0.01912 =
0.01848 0.00092 0.00112 0.00050
N3 5 0.395202 0.720423 0.314351 11.00000 0.02265 0.01957 =
0.01688 -0.00080 0.00384 -0.00066
C1 1 0.550159 0.923700 0.255051 11.00000 0.02685 0.01503 =
0.01957 -0.00033 0.00118 -0.00239
C2 1 0.692958 0.906409 0.229193 11.00000 0.02669 0.02115 =
0.02053 -0.00353 0.00026 -0.00251
C3 1 0.745401 0.959831 0.160013 11.00000 0.03056 0.02728 =
0.02573 -0.00336 0.00569 -0.00509
AFIX 43
H3 2 0.842103 0.948778 0.143488 11.00000 -1.20000
AFIX 0
C4 1 0.662898 1.028633 0.113937 11.00000 0.05167 0.02143 =
0.02328 0.00031 0.00325 -0.00977
C5 1 0.522115 1.043717 0.139728 11.00000 0.04664 0.02136 =
0.02602 0.00479 -0.00731 0.00122
AFIX 43
H5 2 0.463086 1.090024 0.108817 11.00000 -1.20000
AFIX 0
C6 1 0.465189 0.993628 0.208791 11.00000 0.03290 0.01684 =
0.02685 0.00026 -0.00503 -0.00035
C7 1 0.312873 1.019451 0.233800 11.00000 0.03417 0.02851 =
0.04007 0.00705 -0.00434 0.00989
AFIX 137
H7A 2 0.252673 0.949921 0.239037 11.00000 -1.50000
H7B 2 0.269646 1.064751 0.191702 11.00000 -1.50000
H7C 2 0.317759 1.060388 0.286843 11.00000 -1.50000
AFIX 0
C8 1 0.721420 1.085731 0.038753 11.00000 0.07028 0.03728 =
0.03079 0.00936 0.01130 -0.00620
AFIX 137
H8A 2 0.727836 1.166351 0.048804 11.00000 -1.50000
H8B 2 0.655924 1.066860 -0.008601 11.00000 -1.50000
H8C 2 0.818600 1.061156 0.027108 11.00000 -1.50000
AFIX 0
C9 1 0.791075 0.831661 0.273618 11.00000 0.02537 0.03349 =
0.03036 0.00067 0.00564 0.00722
AFIX 137
H9A 2 0.842163 0.873343 0.319329 11.00000 -1.50000
H9B 2 0.862485 0.804501 0.235169 11.00000 -1.50000
H9C 2 0.732489 0.768450 0.295292 11.00000 -1.50000
AFIX 0
C10 1 0.614654 0.857479 0.435568 11.00000 0.02291 0.02353 =
0.01829 -0.00442 0.00236 0.00249
C11 1 0.638796 0.764548 0.484110 11.00000 0.02591 0.02553 =
0.01981 -0.00198 0.00506 0.00471
C12 1 0.746949 0.775144 0.545622 11.00000 0.02953 0.03544 =
0.01988 0.00274 0.00533 0.00793
AFIX 43
H12 2 0.763510 0.712557 0.578075 11.00000 -1.20000
AFIX 0
C13 1 0.831115 0.872736 0.561439 11.00000 0.02429 0.04441 =
0.01879 -0.00291 0.00407 0.00234
C14 1 0.799426 0.964512 0.516890 11.00000 0.02835 0.03205 =
0.02515 -0.00804 0.00528 -0.00553
AFIX 43
H14 2 0.853220 1.033292 0.528453 11.00000 -1.20000
AFIX 0
C15 1 0.690877 0.959287 0.455459 11.00000 0.02717 0.02543 =
0.01950 -0.00201 0.00699 0.00142
C16 1 0.657808 1.066055 0.414209 11.00000 0.03508 0.02293 =
0.03136 -0.00470 0.00191 -0.00241
AFIX 137
H16A 2 0.702077 1.129506 0.446724 11.00000 -1.50000
H16B 2 0.551989 1.071366 0.410548 11.00000 -1.50000
H16C 2 0.697930 1.066481 0.358623 11.00000 -1.50000
AFIX 0
C17 1 0.951954 0.877693 0.626277 11.00000 0.03195 0.06509 =
0.03324 0.00231 -0.00466 -0.00140
AFIX 137
H17A 2 0.914974 0.844663 0.677051 11.00000 -1.50000
H17B 2 0.986225 0.955326 0.637614 11.00000 -1.50000
H17C 2 1.032934 0.836300 0.606163 11.00000 -1.50000
AFIX 0
C18 1 0.549430 0.655935 0.475628 11.00000 0.04532 0.02475 =
0.03065 0.00807 -0.00496 0.00100
AFIX 137
H18A 2 0.590287 0.601757 0.512013 11.00000 -1.50000
H18B 2 0.551002 0.628331 0.418323 11.00000 -1.50000
H18C 2 0.448671 0.666822 0.491012 11.00000 -1.50000
AFIX 0
C19 1 0.333266 0.488316 0.171221 11.00000 0.02595 0.02193 =
0.01665 0.00072 0.00667 -0.00183
C20 1 0.267336 0.386173 0.127268 11.00000 0.03142 0.01967 =
0.02626 -0.00132 -0.00608 0.00090
C21 1 0.159173 0.320274 0.165607 11.00000 0.03676 0.02703 =
0.03291 0.00229 -0.00854 -0.00029
AFIX 43
H21 2 0.128431 0.339961 0.219321 11.00000 -1.20000
AFIX 0
C22 1 0.096795 0.225865 0.124848 11.00000 0.04090 0.02490 =
0.06086 0.00890 -0.02130 -0.00443
AFIX 43
H22 2 0.022604 0.180937 0.150400 11.00000 -1.20000
AFIX 0
C23 1 0.143030 0.197309 0.046770 11.00000 0.05955 0.02268 =
0.06327 -0.01093 -0.03314 0.01049
AFIX 43
H23 2 0.100706 0.132401 0.019039 11.00000 -1.20000
AFIX 0
C24 1 0.249204 0.261914 0.009315 11.00000 0.05608 0.03781 =
0.03959 -0.01509 -0.01695 0.01885
AFIX 43
H24 2 0.280421 0.241793 -0.044212 11.00000 -1.20000
AFIX 0
C25 1 0.310726 0.356026 0.049217 11.00000 0.04141 0.03125 =
0.03007 -0.00643 -0.00592 0.00799
AFIX 43
H25 2 0.383949 0.400832 0.022767 11.00000 -1.20000
AFIX 0
C26 1 0.560824 0.411598 0.233502 11.00000 0.02331 0.02672 =
0.02887 -0.00373 0.00239 0.00640
C27 1 0.642294 0.389138 0.154737 11.00000 0.03170 0.05223 =
0.03809 -0.00845 0.00780 0.01264
AFIX 137
H27A 2 0.576134 0.348936 0.114556 11.00000 -1.50000
H27B 2 0.724507 0.344184 0.167111 11.00000 -1.50000
H27C 2 0.678774 0.459811 0.131757 11.00000 -1.50000
AFIX 0
C28 1 0.491471 0.304008 0.266015 11.00000 0.03868 0.03070 =
0.05182 0.01056 0.00117 0.01006
AFIX 137
H28A 2 0.433322 0.320393 0.314340 11.00000 -1.50000
H28B 2 0.567987 0.255356 0.281718 11.00000 -1.50000
H28C 2 0.428335 0.266826 0.222973 11.00000 -1.50000
AFIX 0
C29 1 0.668465 0.463968 0.298130 11.00000 0.03600 0.04125 =
0.04323 -0.00879 -0.00929 0.01456
AFIX 137
H29A 2 0.709735 0.535417 0.278696 11.00000 -1.50000
H29B 2 0.747021 0.414346 0.307285 11.00000 -1.50000
H29C 2 0.617848 0.475815 0.349964 11.00000 -1.50000
AFIX 0
C30 1 0.153688 0.627663 0.123150 11.00000 0.02715 0.02569 =
0.01834 0.00164 -0.00047 0.00136
C31 1 0.159086 0.605588 0.029883 11.00000 0.04164 0.03411 =
0.02280 -0.00066 -0.00456 0.00811
AFIX 137
H31A 2 0.251519 0.637798 0.009001 11.00000 -1.50000
H31B 2 0.077772 0.639565 0.002614 11.00000 -1.50000
H31C 2 0.151420 0.525276 0.018347 11.00000 -1.50000
AFIX 0
C32 1 0.159079 0.752510 0.140181 11.00000 0.03564 0.02756 =
0.02301 0.00465 -0.00019 0.00491
AFIX 137
H32A 2 0.150858 0.767118 0.199577 11.00000 -1.50000
H32B 2 0.078096 0.784026 0.110767 11.00000 -1.50000
H32C 2 0.251754 0.786767 0.121164 11.00000 -1.50000
AFIX 0
C33 1 0.013486 0.574881 0.158656 11.00000 0.02622 0.03082 =
0.03525 0.00566 0.00076 0.00211
AFIX 137
H33A 2 0.005861 0.495027 0.145274 11.00000 -1.50000
H33B 2 -0.070622 0.609291 0.134766 11.00000 -1.50000
H33C 2 0.015268 0.586461 0.218708 11.00000 -1.50000
AFIX 0
C34 1 0.261982 0.676744 0.348409 11.00000 0.02166 0.02550 =
0.01385 0.00092 0.00141 0.00025
C35 1 0.148984 0.743257 0.368407 11.00000 0.02631 0.02519 =
0.02199 0.00302 0.00217 0.00168
AFIX 43
H35 2 0.160440 0.820861 0.359544 11.00000 -1.20000
AFIX 0
C36 1 0.020161 0.698729 0.400958 11.00000 0.02355 0.04098 =
0.02426 0.00287 0.00415 0.00590
AFIX 43
H36 2 -0.053907 0.746437 0.415559 11.00000 -1.20000
AFIX 0
C37 1 -0.001661 0.586788 0.412333 11.00000 0.02368 0.04468 =
0.02213 0.00987 0.00440 -0.00307
AFIX 43
H37 2 -0.090990 0.556375 0.433469 11.00000 -1.20000
AFIX 0
C38 1 0.109019 0.518483 0.392443 11.00000 0.03449 0.02993 =
0.02627 0.00770 0.00483 -0.00298
AFIX 43
H38 2 0.094967 0.440598 0.399498 11.00000 -1.20000
AFIX 0
C39 1 0.240127 0.563236 0.362305 11.00000 0.02719 0.02624 =
0.01820 0.00252 0.00466 0.00156
AFIX 43
H39 2 0.316125 0.515788 0.350974 11.00000 -1.20000
AFIX 0
HKLF 4
REM 2-XCD430 in P-1
REM wR2 = 0.0577, GooF = S = 0.879, Restrained GooF = 0.880 for all data
REM R1 = 0.0278 for 6232 Fo > 4sig(Fo) and 0.0541 for all 9516 data
REM 409 parameters refined using 12 restraints
END
WGHT 0.0268 0.0000
REM Highest difference peak 0.399, deepest hole -0.425, 1-sigma level 0.058
Q1 1 0.4234 0.7862 0.3392 11.00000 0.05 0.40
Q2 1 0.1594 0.6274 0.0787 11.00000 0.05 0.35
Q3 1 0.4077 0.9133 0.3929 11.00000 0.05 0.34
Q4 1 0.1030 0.7094 0.3956 11.00000 0.05 0.34
Q5 1 0.4260 0.7156 0.2608 11.00000 0.05 0.32
Q6 1 0.7978 1.1520 0.0586 11.00000 0.05 0.31
Q7 1 0.5090 0.7391 0.2219 11.00000 0.05 0.31
Q8 1 0.5396 0.8655 0.4108 11.00000 0.05 0.30
Q9 1 0.7477 1.0206 -0.0010 11.00000 0.05 0.29
Q10 1 0.7137 0.9625 0.4980 11.00000 0.05 0.27
;
_shelx_res_checksum 35275
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_xcd155
_database_code_depnum_ccdc_archive 'CCDC 1922575'
loop_
_audit_author_name
_audit_author_address
'Michael T. Gamer'
;Karlsruhe Institute of Technology
Germany
;
_audit_update_record
;
2019-06-12 deposited with the CCDC. 2019-07-05 downloaded from the CCDC.
;
_audit_creation_date 2019-03-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number 2018/3
#==============================================================================
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C48 H54 As2 Cl2 Ge2 N2, C5 H12'
_chemical_formula_sum 'C53 H66 As2 Cl2 Ge2 N2'
_chemical_formula_weight 1096.99
_chemical_melting_point ?
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'
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'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/c 1'
_space_group_name_Hall '-P 2ybc'
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'
_cell_length_a 12.3661(12)
_cell_length_b 8.5420(5)
_cell_length_c 24.170(2)
_cell_angle_alpha 90
_cell_angle_beta 98.891(7)
_cell_angle_gamma 90
_cell_volume 2522.4(4)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 11844
_cell_measurement_temperature 100
_cell_measurement_theta_max 28.96
_cell_measurement_theta_min 2.53
_shelx_estimated_absorpt_T_max 0.893
_shelx_estimated_absorpt_T_min 0.657
_exptl_absorpt_coefficient_mu 2.636
_exptl_absorpt_correction_T_max 0.8928
_exptl_absorpt_correction_T_min 0.4507
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens published in F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270.
Afterwards scaling of reflection intensities was performed within STOE LANA.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol.9, no.2, 2016, pp. 136-140.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'light yellow'
_exptl_crystal_colour_modifier light
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.444
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description needle
_exptl_crystal_F_000 1124
_exptl_crystal_size_max 0.174
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.044
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0475
_diffrn_reflns_av_unetI/netI 0.0838
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.870
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_h_min -16
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 14593
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 29.656
_diffrn_reflns_theta_min 2.532
_diffrn_ambient_temperature 100
_diffrn_detector Pilatus200K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type 'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.870
_diffrn_measurement_device 'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type 'Bruker P4'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_collimation '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_polarisn_norm 0
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'Mo Genix 3D HF'
_diffrn_source_current 1.000
_diffrn_source_power 0.050
_diffrn_source_voltage 50
_diffrn_special_details ?
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3699
_reflns_number_total 6191
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_data_collection 'X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)'
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
PLATON (A.L.Spek, 2009)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
PLATON (A.L.Spek, 2009)
;
_computing_structure_solution 'SHELXS-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)'
_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)
;
_refine_diff_density_max 0.799
_refine_diff_density_min -0.856
_refine_diff_density_rms 0.112
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.983
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 259
_refine_ls_number_reflns 6191
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1009
_refine_ls_R_factor_gt 0.0515
_refine_ls_restrained_S_all 0.983
_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/[\s^2^(Fo^2^)+(0.0616P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1103
_refine_ls_wR_factor_ref 0.1291
_refine_special_details ?
_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:
C5(H5), C21(H21), C20(H20), C24(H24), C14(H14), C3(H3), C12(H12), C22(H22),
C23(H23)
2.b Idealised Me refined as rotating group:
C16(H16A,H16B,H16C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C),
C18(H18A,H18B,H18C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
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
As As 0.26188(4) 0.51334(5) 0.44518(2) 0.02969(14) Uani 1 1 d . . . . .
Ge Ge 0.07699(4) 0.47612(5) 0.46539(2) 0.02795(14) Uani 1 1 d . . . . .
Cl Cl 0.02992(9) 0.30892(12) 0.39670(5) 0.0363(3) Uani 1 1 d . . . . .
N N 0.0393(3) 0.3904(4) 0.52970(15) 0.0310(9) Uani 1 1 d . . . . .
C5 C 0.4247(4) 0.7699(5) 0.58647(18) 0.0318(10) Uani 1 1 d . . . . .
H5 H 0.415382 0.794505 0.623771 0.038 Uiso 1 1 calc R . . . .
C19 C 0.0982(3) 0.2858(5) 0.56725(18) 0.0292(10) Uani 1 1 d . . . . .
C1 C 0.3563(4) 0.6495(5) 0.49842(19) 0.0306(10) Uani 1 1 d . . . . .
C16 C 0.1669(4) 0.8835(5) 0.44720(19) 0.0370(11) Uani 1 1 d . . . . .
H16A H 0.240258 0.905982 0.467377 0.056 Uiso 1 1 calc GR . . . .
H16B H 0.129968 0.809113 0.468849 0.056 Uiso 1 1 calc GR . . . .
H16C H 0.124509 0.980775 0.442039 0.056 Uiso 1 1 calc GR . . . .
C2 C 0.4527(4) 0.6957(5) 0.47781(19) 0.0334(11) Uani 1 1 d . . . . .
C6 C 0.3429(4) 0.6831(5) 0.55295(18) 0.0318(10) Uani 1 1 d . . . . .
C15 C 0.1762(4) 0.8140(5) 0.39091(19) 0.0320(10) Uani 1 1 d . . . . .
C21 C 0.1410(4) 0.1685(5) 0.65892(19) 0.0376(11) Uani 1 1 d . . . . .
H21 H 0.128014 0.160760 0.696547 0.045 Uiso 1 1 calc R . . . .
C20 C 0.0811(4) 0.2740(5) 0.62315(18) 0.0333(10) Uani 1 1 d . . . . .
H20 H 0.028217 0.338720 0.636459 0.040 Uiso 1 1 calc R . . . .
C4 C 0.5178(4) 0.8204(5) 0.56729(19) 0.0340(11) Uani 1 1 d . . . . .
C24 C 0.1776(4) 0.1919(5) 0.54992(19) 0.0363(11) Uani 1 1 d . . . . .
H24 H 0.191588 0.199047 0.512442 0.044 Uiso 1 1 calc R . . . .
C14 C 0.1464(4) 0.9071(5) 0.3436(2) 0.0375(12) Uani 1 1 d . . . . .
H14 H 0.124601 1.012013 0.348777 0.045 Uiso 1 1 calc R . . . .
C11 C 0.2140(4) 0.6027(5) 0.32862(19) 0.0331(11) Uani 1 1 d . . . . .
C3 C 0.5302(4) 0.7825(5) 0.51339(19) 0.0347(11) Uani 1 1 d . . . . .
H3 H 0.594222 0.816761 0.499714 0.042 Uiso 1 1 calc R . . . .
C10 C 0.2110(4) 0.6590(5) 0.38292(19) 0.0334(11) Uani 1 1 d . . . . .
C13 C 0.1472(4) 0.8544(5) 0.28982(19) 0.0396(12) Uani 1 1 d . . . . .
C8 C 0.4775(4) 0.6521(5) 0.42115(19) 0.0369(11) Uani 1 1 d . . . . .
H8A H 0.470228 0.538586 0.416069 0.055 Uiso 1 1 calc GR . . . .
H8B H 0.552455 0.683841 0.417980 0.055 Uiso 1 1 calc GR . . . .
H8C H 0.426093 0.705385 0.392299 0.055 Uiso 1 1 calc GR . . . .
C7 C 0.2451(4) 0.6329(6) 0.5778(2) 0.0460(13) Uani 1 1 d . . . . .
H7A H 0.240764 0.518333 0.577652 0.069 Uiso 1 1 calc GR . . . .
H7B H 0.178795 0.676081 0.555586 0.069 Uiso 1 1 calc GR . . . .
H7C H 0.251655 0.671296 0.616345 0.069 Uiso 1 1 calc GR . . . .
C12 C 0.1815(4) 0.7007(5) 0.2832(2) 0.0405(12) Uani 1 1 d . . . . .
H12 H 0.182634 0.661865 0.246422 0.049 Uiso 1 1 calc R . . . .
C22 C 0.2194(4) 0.0741(6) 0.6410(2) 0.0426(12) Uani 1 1 d . . . . .
H22 H 0.259967 0.001607 0.665791 0.051 Uiso 1 1 calc R . . . .
C23 C 0.2374(4) 0.0870(5) 0.5867(2) 0.0435(13) Uani 1 1 d . . . . .
H23 H 0.291546 0.023410 0.573958 0.052 Uiso 1 1 calc R . . . .
C9 C 0.6032(4) 0.9134(5) 0.6043(2) 0.0447(13) Uani 1 1 d . . . . .
H9A H 0.604952 1.020372 0.589772 0.067 Uiso 1 1 calc GR . . . .
H9B H 0.674916 0.864272 0.604778 0.067 Uiso 1 1 calc GR . . . .
H9C H 0.585347 0.916282 0.642374 0.067 Uiso 1 1 calc GR . . . .
C18 C 0.2525(4) 0.4396(5) 0.3172(2) 0.0421(12) Uani 1 1 d . . . . .
H18A H 0.325204 0.421943 0.338963 0.063 Uiso 1 1 calc GR . . . .
H18B H 0.256377 0.428569 0.277235 0.063 Uiso 1 1 calc GR . . . .
H18C H 0.200966 0.362650 0.328141 0.063 Uiso 1 1 calc GR . . . .
C17 C 0.1136(5) 0.9583(6) 0.2404(2) 0.0585(16) Uani 1 1 d . . . . .
H17A H 0.040202 0.928847 0.222061 0.088 Uiso 1 1 calc GR . . . .
H17B H 0.165618 0.946700 0.213944 0.088 Uiso 1 1 calc GR . . . .
H17C H 0.113087 1.067379 0.252918 0.088 Uiso 1 1 calc GR . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
As 0.0291(3) 0.0265(2) 0.0327(3) -0.00076(19) 0.00228(19) 0.00321(19)
Ge 0.0284(3) 0.0241(2) 0.0306(3) -0.00001(19) 0.00229(19) 0.00260(19)
Cl 0.0362(7) 0.0334(6) 0.0382(6) -0.0086(5) 0.0023(5) 0.0011(5)
N 0.032(2) 0.0245(18) 0.036(2) 0.0001(16) 0.0022(17) 0.0053(15)
C5 0.036(3) 0.028(2) 0.029(2) 0.0045(19) -0.002(2) 0.005(2)
C19 0.026(2) 0.025(2) 0.035(3) 0.0023(19) -0.0009(19) 0.0014(18)
C1 0.030(3) 0.022(2) 0.037(3) -0.0020(18) -0.005(2) 0.0032(18)
C16 0.036(3) 0.026(2) 0.048(3) -0.002(2) 0.005(2) 0.004(2)
C2 0.031(3) 0.025(2) 0.041(3) 0.003(2) -0.004(2) 0.0083(19)
C6 0.033(3) 0.026(2) 0.035(3) 0.0038(19) 0.001(2) 0.0032(19)
C15 0.028(3) 0.028(2) 0.039(3) 0.003(2) 0.004(2) -0.0026(19)
C21 0.035(3) 0.043(3) 0.032(3) 0.011(2) -0.003(2) 0.009(2)
C20 0.031(3) 0.032(2) 0.037(3) -0.001(2) 0.005(2) 0.007(2)
C4 0.035(3) 0.026(2) 0.039(3) 0.005(2) -0.001(2) 0.0041(19)
C24 0.042(3) 0.034(2) 0.033(3) 0.003(2) 0.008(2) 0.005(2)
C14 0.035(3) 0.024(2) 0.049(3) 0.000(2) -0.004(2) -0.002(2)
C11 0.028(3) 0.037(3) 0.032(3) 0.000(2) 0.001(2) -0.004(2)
C3 0.026(3) 0.035(2) 0.042(3) 0.004(2) 0.002(2) -0.003(2)
C10 0.034(3) 0.031(2) 0.034(3) -0.0009(19) 0.003(2) 0.003(2)
C13 0.039(3) 0.042(3) 0.034(3) 0.003(2) -0.005(2) 0.001(2)
C8 0.030(3) 0.035(2) 0.045(3) 0.002(2) 0.006(2) 0.004(2)
C7 0.042(3) 0.058(3) 0.038(3) -0.010(2) 0.007(2) -0.006(3)
C12 0.044(3) 0.046(3) 0.031(3) -0.004(2) 0.004(2) -0.006(2)
C22 0.045(3) 0.043(3) 0.039(3) 0.016(2) 0.003(2) 0.018(2)
C23 0.049(3) 0.031(2) 0.049(3) 0.004(2) 0.001(2) 0.017(2)
C9 0.042(3) 0.037(3) 0.052(3) 0.001(2) -0.003(3) -0.006(2)
C18 0.044(3) 0.040(3) 0.043(3) -0.006(2) 0.006(2) 0.007(2)
C17 0.070(4) 0.062(3) 0.039(3) 0.010(3) -0.005(3) 0.006(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
As Ge 2.4316(7) . ?
As C1 1.976(4) . ?
As C10 1.979(4) . ?
Ge Ge 2.7523(10) 3_566 ?
Ge Cl 2.1992(12) . ?
Ge N 1.853(3) 3_566 ?
Ge N 1.842(4) . ?
N C19 1.396(5) . ?
C5 C6 1.406(6) . ?
C5 C4 1.375(6) . ?
C19 C20 1.403(6) . ?
C19 C24 1.382(6) . ?
C1 C2 1.417(6) . ?
C1 C6 1.384(6) . ?
C16 C15 1.505(6) . ?
C2 C3 1.398(6) . ?
C2 C8 1.496(6) . ?
C6 C7 1.493(6) . ?
C15 C14 1.394(6) . ?
C15 C10 1.414(6) . ?
C21 C20 1.382(5) . ?
C21 C22 1.381(6) . ?
C4 C3 1.374(6) . ?
C4 C9 1.501(6) . ?
C24 C23 1.392(6) . ?
C14 C13 1.377(6) . ?
C11 C10 1.404(6) . ?
C11 C12 1.390(6) . ?
C11 C18 1.510(6) . ?
C13 C12 1.397(6) . ?
C13 C17 1.493(6) . ?
C22 C23 1.368(7) . ?
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 As Ge 115.16(14) . . ?
C1 As C10 102.20(18) . . ?
C10 As Ge 92.11(14) . . ?
As Ge Ge 149.66(3) . 3_566 ?
Cl Ge As 94.62(4) . . ?
Cl Ge Ge 115.33(4) . 3_566 ?
N Ge As 126.16(11) . . ?
N Ge As 134.06(11) 3_566 . ?
N Ge Ge 42.00(10) . 3_566 ?
N Ge Ge 41.70(11) 3_566 3_566 ?
N Ge Cl 109.29(11) 3_566 . ?
N Ge Cl 107.88(11) . . ?
N Ge N 83.71(16) . 3_566 ?
Ge N Ge 96.29(15) . 3_566 ?
C19 N Ge 128.9(3) . . ?
C19 N Ge 133.2(3) . 3_566 ?
C4 C5 C6 122.5(4) . . ?
N C19 C20 122.1(4) . . ?
C24 C19 N 119.9(4) . . ?
C24 C19 C20 118.0(4) . . ?
C2 C1 As 112.3(3) . . ?
C6 C1 As 126.6(4) . . ?
C6 C1 C2 120.5(4) . . ?
C1 C2 C8 123.7(4) . . ?
C3 C2 C1 117.8(4) . . ?
C3 C2 C8 118.5(4) . . ?
C5 C6 C7 118.4(4) . . ?
C1 C6 C5 118.5(4) . . ?
C1 C6 C7 123.1(4) . . ?
C14 C15 C16 118.0(4) . . ?
C14 C15 C10 118.0(4) . . ?
C10 C15 C16 124.1(4) . . ?
C22 C21 C20 121.2(5) . . ?
C21 C20 C19 120.2(4) . . ?
C5 C4 C9 120.9(4) . . ?
C3 C4 C5 117.9(4) . . ?
C3 C4 C9 121.2(4) . . ?
C19 C24 C23 120.8(4) . . ?
C13 C14 C15 123.3(4) . . ?
C10 C11 C18 122.8(4) . . ?
C12 C11 C10 119.1(4) . . ?
C12 C11 C18 118.2(4) . . ?
C4 C3 C2 122.8(4) . . ?
C15 C10 As 123.5(3) . . ?
C11 C10 As 116.3(3) . . ?
C11 C10 C15 120.1(4) . . ?
C14 C13 C12 117.5(4) . . ?
C14 C13 C17 121.3(4) . . ?
C12 C13 C17 121.2(5) . . ?
C11 C12 C13 122.1(4) . . ?
C23 C22 C21 118.7(4) . . ?
C22 C23 C24 121.0(5) . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 -0.846 0.250 214.1 47.0 ?
2 0.500 -0.430 0.750 214.1 47.0 ?
_shelx_res_file
;
TITL 3-XCD155 in P2(1)/c
xcd155.res
created by SHELXL-2018/3 at 16:44:17 on 11-Mar-2019
CELL 0.71073 12.3661 8.542 24.1698 90 98.891 90
ZERR 2 0.0012 0.0005 0.0022 0 0.007 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H As Cl Ge N
UNIT 106 132 4 4 4 4
L.S. 10 0 0
PLAN 10
SIZE 0.044 0.09 0.174
TEMP -173.15
BOND
LIST 4
fmap 2 52
acta 52
ABIN
REM
REM
REM
WGHT 0.061600
FVAR 0.33362
AS 3 0.261878 0.513337 0.445176 11.00000 0.02907 0.02654 =
0.03268 -0.00076 0.00228 0.00321
GE 5 0.076990 0.476118 0.465393 11.00000 0.02839 0.02415 =
0.03061 -0.00001 0.00229 0.00260
CL 4 0.029921 0.308918 0.396697 11.00000 0.03616 0.03340 =
0.03817 -0.00859 0.00233 0.00113
N 6 0.039274 0.390422 0.529700 11.00000 0.03163 0.02450 =
0.03587 0.00011 0.00223 0.00530
C5 1 0.424721 0.769876 0.586472 11.00000 0.03609 0.02813 =
0.02912 0.00448 -0.00155 0.00496
AFIX 43
H5 2 0.415382 0.794505 0.623771 11.00000 -1.20000
AFIX 0
C19 1 0.098204 0.285842 0.567245 11.00000 0.02601 0.02540 =
0.03454 0.00229 -0.00093 0.00144
C1 1 0.356262 0.649464 0.498416 11.00000 0.03030 0.02178 =
0.03657 -0.00203 -0.00465 0.00317
C16 1 0.166916 0.883528 0.447204 11.00000 0.03595 0.02630 =
0.04831 -0.00247 0.00478 0.00430
AFIX 137
H16A 2 0.240258 0.905982 0.467377 11.00000 -1.50000
H16B 2 0.129968 0.809113 0.468849 11.00000 -1.50000
H16C 2 0.124509 0.980775 0.442039 11.00000 -1.50000
AFIX 0
C2 1 0.452650 0.695736 0.477808 11.00000 0.03130 0.02532 =
0.04071 0.00334 -0.00379 0.00829
C6 1 0.342866 0.683086 0.552954 11.00000 0.03292 0.02640 =
0.03471 0.00385 0.00054 0.00317
C15 1 0.176151 0.813978 0.390912 11.00000 0.02792 0.02847 =
0.03916 0.00305 0.00401 -0.00260
C21 1 0.140996 0.168497 0.658917 11.00000 0.03534 0.04258 =
0.03229 0.01108 -0.00307 0.00856
AFIX 43
H21 2 0.128014 0.160760 0.696547 11.00000 -1.20000
AFIX 0
C20 1 0.081131 0.273985 0.623149 11.00000 0.03125 0.03180 =
0.03663 -0.00067 0.00488 0.00706
AFIX 43
H20 2 0.028217 0.338720 0.636459 11.00000 -1.20000
AFIX 0
C4 1 0.517771 0.820436 0.567291 11.00000 0.03452 0.02596 =
0.03930 0.00463 -0.00114 0.00405
C24 1 0.177631 0.191908 0.549923 11.00000 0.04195 0.03448 =
0.03319 0.00325 0.00791 0.00463
AFIX 43
H24 2 0.191588 0.199047 0.512442 11.00000 -1.20000
AFIX 0
C14 1 0.146435 0.907059 0.343632 11.00000 0.03531 0.02442 =
0.04936 0.00020 -0.00414 -0.00225
AFIX 43
H14 2 0.124601 1.012013 0.348777 11.00000 -1.20000
AFIX 0
C11 1 0.214043 0.602652 0.328618 11.00000 0.02822 0.03748 =
0.03241 0.00027 0.00071 -0.00390
C3 1 0.530195 0.782526 0.513387 11.00000 0.02631 0.03512 =
0.04178 0.00392 0.00240 -0.00330
AFIX 43
H3 2 0.594222 0.816761 0.499714 11.00000 -1.20000
AFIX 0
C10 1 0.211026 0.659040 0.382922 11.00000 0.03409 0.03131 =
0.03403 -0.00087 0.00291 0.00316
C13 1 0.147160 0.854408 0.289824 11.00000 0.03873 0.04249 =
0.03401 0.00289 -0.00540 0.00125
C8 1 0.477499 0.652126 0.421153 11.00000 0.03027 0.03492 =
0.04536 0.00214 0.00568 0.00425
AFIX 137
H8A 2 0.470228 0.538586 0.416069 11.00000 -1.50000
H8B 2 0.552455 0.683841 0.417980 11.00000 -1.50000
H8C 2 0.426093 0.705385 0.392299 11.00000 -1.50000
AFIX 0
C7 1 0.245127 0.632888 0.577765 11.00000 0.04217 0.05837 =
0.03778 -0.00956 0.00694 -0.00647
AFIX 137
H7A 2 0.240764 0.518333 0.577652 11.00000 -1.50000
H7B 2 0.178795 0.676081 0.555586 11.00000 -1.50000
H7C 2 0.251655 0.671296 0.616345 11.00000 -1.50000
AFIX 0
C12 1 0.181493 0.700660 0.283164 11.00000 0.04417 0.04582 =
0.03083 -0.00383 0.00396 -0.00608
AFIX 43
H12 2 0.182634 0.661865 0.246422 11.00000 -1.20000
AFIX 0
C22 1 0.219375 0.074092 0.640956 11.00000 0.04521 0.04304 =
0.03862 0.01597 0.00314 0.01770
AFIX 43
H22 2 0.259967 0.001607 0.665791 11.00000 -1.20000
AFIX 0
C23 1 0.237394 0.087020 0.586713 11.00000 0.04924 0.03065 =
0.04866 0.00382 0.00146 0.01654
AFIX 43
H23 2 0.291546 0.023410 0.573958 11.00000 -1.20000
AFIX 0
C9 1 0.603153 0.913406 0.604261 11.00000 0.04224 0.03710 =
0.05161 0.00108 -0.00315 -0.00624
AFIX 137
H9A 2 0.604952 1.020372 0.589772 11.00000 -1.50000
H9B 2 0.674916 0.864272 0.604778 11.00000 -1.50000
H9C 2 0.585347 0.916282 0.642374 11.00000 -1.50000
AFIX 0
C18 1 0.252526 0.439642 0.317240 11.00000 0.04359 0.03964 =
0.04295 -0.00628 0.00591 0.00690
AFIX 137
H18A 2 0.325204 0.421943 0.338963 11.00000 -1.50000
H18B 2 0.256377 0.428569 0.277235 11.00000 -1.50000
H18C 2 0.200966 0.362650 0.328141 11.00000 -1.50000
AFIX 0
C17 1 0.113635 0.958260 0.240442 11.00000 0.07045 0.06161 =
0.03924 0.01023 -0.00475 0.00574
AFIX 137
H17A 2 0.040202 0.928847 0.222061 11.00000 -1.50000
H17B 2 0.165618 0.946700 0.213944 11.00000 -1.50000
H17C 2 0.113087 1.067379 0.252918 11.00000 -1.50000
AFIX 0
HKLF 4
REM 3-XCD155 in P2(1)/c
REM wR2 = 0.1291, GooF = S = 0.983, Restrained GooF = 0.983 for all data
REM R1 = 0.0515 for 3699 Fo > 4sig(Fo) and 0.1009 for all 6191 data
REM 259 parameters refined using 0 restraints
END
WGHT 0.0616 0.0000
REM Highest difference peak 0.799, deepest hole -0.856, 1-sigma level 0.112
Q1 1 0.1675 0.5238 0.4580 11.00000 0.05 0.80
Q2 1 -0.0019 0.3798 0.4436 11.00000 0.05 0.53
Q3 1 0.2510 0.6145 0.4220 11.00000 0.05 0.52
Q4 1 0.2764 0.6207 0.4595 11.00000 0.05 0.51
Q5 1 0.0198 0.5008 0.5195 11.00000 0.05 0.50
Q6 1 0.2274 0.5159 0.3202 11.00000 0.05 0.50
Q7 1 0.0860 0.5863 0.4643 11.00000 0.05 0.50
Q8 1 0.0212 0.4850 0.5531 11.00000 0.05 0.49
Q9 1 0.3339 0.5752 0.4776 11.00000 0.05 0.47
Q10 1 0.0787 0.3826 0.4776 11.00000 0.05 0.47
;
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16 1 5 0.1884 -0.0619
0 0 0 0.0 0.0
;
_shelx_fab_checksum 27260
_olex2_submission_special_instructions 'No special instructions were received'