#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:01:33 +0300 (Sat, 05 Jun 2021) $
#$Revision: 265933 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/08/1560843.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1560843
loop_
_publ_author_name
'Keil, Philip M.'
'Szilvási, Tibor'
'Hadlington, Terrance J.'
_publ_section_title
;
 Reversible metathesis of ammonia in an acyclic germylene--Ni0 complex
;
_journal_issue                   15
_journal_name_full               'Chemical Science'
_journal_page_first              5582
_journal_page_last               5590
_journal_paper_doi               10.1039/D1SC00450F
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C37 H39 Cl Ge N P Si'
_chemical_formula_sum            'C37 H39 Cl Ge N P Si'
_chemical_formula_weight         664.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-01-19 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                96.00(3)
_cell_angle_beta                 93.00(3)
_cell_angle_gamma                109.00(3)
_cell_formula_units_Z            2
_cell_length_a                   11.000(2)
_cell_length_b                   12.100(2)
_cell_length_c                   13.500(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.50
_cell_measurement_theta_min      1.92
_cell_volume                     1682.5(7)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16730
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         3.047
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.515
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         6600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0525P)²+0.5403P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0855
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5791
_reflns_number_total             6600
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc00450f2.cif
_cod_data_source_block           compound_1a
_cod_depositor_comments
'Adding full bibliography for 1560843--1560857.cif.'
_cod_database_code               1560843
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.49753(2) 0.58821(2) 0.11920(2) 0.02329(7) Uani 1 1 d . . . . .
Cl1 Cl 0.27630(5) 0.50889(4) 0.13601(4) 0.03137(12) Uani 1 1 d . . . . .
P1 P 0.52140(5) 0.43512(4) 0.21676(4) 0.02279(11) Uani 1 1 d . . . . .
Si1 Si 0.54160(5) 0.65414(4) 0.36147(4) 0.02160(12) Uani 1 1 d . . . . .
N1 N 0.55751(15) 0.69304(13) 0.24231(12) 0.0221(3) Uani 1 1 d . . . . .
C1 C 0.62147(18) 0.81358(16) 0.22633(14) 0.0235(4) Uani 1 1 d . . . . .
C32 C 0.68370(19) 0.42850(17) 0.21814(15) 0.0264(4) Uani 1 1 d . . . . .
C6 C 0.75433(19) 0.85234(18) 0.21272(14) 0.0273(4) Uani 1 1 d . . . . .
C13 C 0.41021(19) 0.69371(17) 0.42642(14) 0.0255(4) Uani 1 1 d . . . . .
C19 C 0.69482(18) 0.72588(18) 0.44621(14) 0.0270(4) Uani 1 1 d . . . . .
C26 C 0.41125(19) 0.28715(17) 0.17594(15) 0.0266(4) Uani 1 1 d . . . . .
C25 C 0.49334(19) 0.48677(16) 0.34172(14) 0.0253(4) Uani 1 1 d . . . . .
H25A H 0.544067 0.461075 0.391671 0.030 Uiso 1 1 calc R U . . .
H25B H 0.400797 0.451570 0.351732 0.030 Uiso 1 1 calc R U . . .
C2 C 0.5497(2) 0.89185(17) 0.22075(14) 0.0273(4) Uani 1 1 d . . . . .
C33 C 0.7469(2) 0.4484(2) 0.13135(17) 0.0355(5) Uani 1 1 d . . . . .
H33 H 0.705606 0.466743 0.074848 0.043 Uiso 1 1 calc R U . . .
C10 C 0.83337(19) 0.76929(19) 0.20527(16) 0.0303(4) Uani 1 1 d . . . . .
H10 H 0.778681 0.691699 0.223507 0.036 Uiso 1 1 calc R U . . .
C7 C 0.4038(2) 0.84970(19) 0.22287(16) 0.0313(4) Uani 1 1 d . . . . .
H7 H 0.378519 0.773288 0.251493 0.038 Uiso 1 1 calc R U . . .
C5 C 0.8136(2) 0.97001(19) 0.20027(16) 0.0334(5) Uani 1 1 d . . . . .
H5 H 0.903489 0.997525 0.192491 0.040 Uiso 1 1 calc R U . . .
C37 C 0.7464(2) 0.4024(2) 0.29979(17) 0.0367(5) Uani 1 1 d . . . . .
H37 H 0.704006 0.387290 0.358960 0.044 Uiso 1 1 calc R U . . .
C24 C 0.7451(2) 0.8495(2) 0.46877(16) 0.0332(5) Uani 1 1 d . . . . .
H24 H 0.703955 0.896243 0.437196 0.040 Uiso 1 1 calc R U . . .
C20 C 0.7603(2) 0.6612(2) 0.49320(16) 0.0344(5) Uani 1 1 d . . . . .
H20 H 0.729608 0.577625 0.479564 0.041 Uiso 1 1 calc R U . . .
C3 C 0.6144(2) 1.00838(19) 0.20729(16) 0.0331(5) Uani 1 1 d . . . . .
H3 H 0.567236 1.061386 0.203833 0.040 Uiso 1 1 calc R U . . .
C27 C 0.4389(2) 0.22135(18) 0.09419(15) 0.0314(4) Uani 1 1 d . . . . .
H27 H 0.520922 0.248569 0.068770 0.038 Uiso 1 1 calc R U . . .
C14 C 0.2801(2) 0.6378(2) 0.39021(16) 0.0322(5) Uani 1 1 d . . . . .
H14 H 0.257906 0.573492 0.338228 0.039 Uiso 1 1 calc R U . . .
C18 C 0.4376(2) 0.78593(19) 0.50561(16) 0.0326(5) Uani 1 1 d . . . . .
H18 H 0.524153 0.823093 0.534038 0.039 Uiso 1 1 calc R U . . .
C4 C 0.7455(2) 1.04826(18) 0.19888(17) 0.0362(5) Uani 1 1 d . . . . .
H4 H 0.788834 1.128653 0.192199 0.043 Uiso 1 1 calc R U . . .
C8 C 0.3567(2) 0.9358(2) 0.28986(18) 0.0389(5) Uani 1 1 d . . . . .
H8A H 0.401217 0.950474 0.357180 0.058 Uiso 1 1 calc R U . . .
H8B H 0.263393 0.901281 0.293487 0.058 Uiso 1 1 calc R U . . .
H8C H 0.375498 1.010231 0.261512 0.058 Uiso 1 1 calc R U . . .
C17 C 0.3402(2) 0.8239(2) 0.54325(18) 0.0418(6) Uani 1 1 d . . . . .
H17 H 0.361123 0.887754 0.595631 0.050 Uiso 1 1 calc R U . . .
C23 C 0.8533(2) 0.9048(2) 0.53612(17) 0.0417(6) Uani 1 1 d . . . . .
H23 H 0.884034 0.988236 0.551046 0.050 Uiso 1 1 calc R U . . .
C34 C 0.8701(2) 0.4414(2) 0.1276(2) 0.0446(6) Uani 1 1 d . . . . .
H34 H 0.912013 0.453245 0.067868 0.054 Uiso 1 1 calc R U . . .
C15 C 0.1832(2) 0.6748(2) 0.42886(17) 0.0381(5) Uani 1 1 d . . . . .
H15 H 0.095719 0.635450 0.403450 0.046 Uiso 1 1 calc R U . . .
C16 C 0.2136(2) 0.7689(2) 0.50449(19) 0.0419(6) Uani 1 1 d . . . . .
H16 H 0.147468 0.795476 0.529527 0.050 Uiso 1 1 calc R U . . .
C35 C 0.9322(2) 0.4173(2) 0.2098(2) 0.0479(6) Uani 1 1 d . . . . .
H35 H 1.017076 0.413971 0.207400 0.057 Uiso 1 1 calc R U . . .
C12 C 0.8654(2) 0.7489(2) 0.09709(18) 0.0392(5) Uani 1 1 d . . . . .
H12A H 0.785144 0.714437 0.053063 0.059 Uiso 1 1 calc R U . . .
H12B H 0.915437 0.695049 0.092751 0.059 Uiso 1 1 calc R U . . .
H12C H 0.916146 0.824335 0.076339 0.059 Uiso 1 1 calc R U . . .
C22 C 0.9162(2) 0.8392(3) 0.58124(18) 0.0492(7) Uani 1 1 d . . . . .
H22 H 0.990725 0.877173 0.626722 0.059 Uiso 1 1 calc R U . . .
C21 C 0.8700(2) 0.7172(3) 0.55980(18) 0.0466(6) Uani 1 1 d . . . . .
H21 H 0.913250 0.671611 0.590628 0.056 Uiso 1 1 calc R U . . .
C29 C 0.2296(2) 0.0754(2) 0.08724(19) 0.0419(6) Uani 1 1 d . . . . .
H29 H 0.166602 0.004071 0.056544 0.050 Uiso 1 1 calc R U . . .
C28 C 0.3476(2) 0.11670(19) 0.04995(17) 0.0381(5) Uani 1 1 d . . . . .
H28 H 0.366634 0.073345 -0.006392 0.046 Uiso 1 1 calc R U . . .
C31 C 0.2935(2) 0.2446(2) 0.21431(19) 0.0407(5) Uani 1 1 d . . . . .
H31 H 0.273934 0.287276 0.270821 0.049 Uiso 1 1 calc R U . . .
C9 C 0.3375(2) 0.8253(2) 0.11620(18) 0.0392(5) Uani 1 1 d . . . . .
H9A H 0.367362 0.896754 0.083544 0.059 Uiso 1 1 calc R U . . .
H9B H 0.243752 0.801728 0.118773 0.059 Uiso 1 1 calc R U . . .
H9C H 0.359052 0.761705 0.078152 0.059 Uiso 1 1 calc R U . . .
C11 C 0.9574(2) 0.8132(2) 0.27649(18) 0.0414(5) Uani 1 1 d . . . . .
H11A H 1.015520 0.886553 0.257264 0.062 Uiso 1 1 calc R U . . .
H11B H 0.999996 0.753431 0.272614 0.062 Uiso 1 1 calc R U . . .
H11C H 0.935896 0.827602 0.345108 0.062 Uiso 1 1 calc R U . . .
C36 C 0.8700(2) 0.3981(3) 0.2955(2) 0.0491(6) Uani 1 1 d . . . . .
H36 H 0.912588 0.381746 0.352376 0.059 Uiso 1 1 calc R U . . .
C30 C 0.2033(2) 0.1384(2) 0.1696(2) 0.0474(6) Uani 1 1 d . . . . .
H30 H 0.122459 0.108955 0.196305 0.057 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
N1 Ge1 Cl1 101.45(6) . . ?
N1 Ge1 P1 85.38(5) . . ?
Cl1 Ge1 P1 86.08(3) . . ?
C32 P1 C26 107.15(9) . . ?
C32 P1 C25 109.28(10) . . ?
C26 P1 C25 110.61(10) . . ?
C32 P1 Ge1 111.31(7) . . ?
C26 P1 Ge1 115.63(7) . . ?
C25 P1 Ge1 102.74(7) . . ?
N1 Si1 C19 112.15(9) . . ?
N1 Si1 C13 114.16(8) . . ?
C19 Si1 C13 106.29(9) . . ?
N1 Si1 C25 103.92(9) . . ?
C19 Si1 C25 112.56(10) . . ?
C13 Si1 C25 107.82(9) . . ?
C1 N1 Si1 121.04(13) . . ?
C1 N1 Ge1 112.73(12) . . ?
Si1 N1 Ge1 126.23(9) . . ?
C6 C1 C2 120.11(18) . . ?
C6 C1 N1 119.82(17) . . ?
C2 C1 N1 120.02(17) . . ?
C37 C32 C33 118.85(19) . . ?
C37 C32 P1 123.41(16) . . ?
C33 C32 P1 117.73(16) . . ?
C5 C6 C1 118.26(19) . . ?
C5 C6 C10 118.91(18) . . ?
C1 C6 C10 122.74(18) . . ?
C14 C13 C18 117.17(19) . . ?
C14 C13 Si1 120.19(15) . . ?
C18 C13 Si1 122.38(16) . . ?
C20 C19 C24 117.0(2) . . ?
C20 C19 Si1 122.73(17) . . ?
C24 C19 Si1 120.23(16) . . ?
C31 C26 C27 119.16(19) . . ?
C31 C26 P1 121.61(16) . . ?
C27 C26 P1 118.63(15) . . ?
P1 C25 Si1 110.85(10) . . ?
C3 C2 C1 118.80(19) . . ?
C3 C2 C7 119.46(19) . . ?
C1 C2 C7 121.63(18) . . ?
C34 C33 C32 120.0(2) . . ?
C6 C10 C11 113.18(18) . . ?
C6 C10 C12 109.92(18) . . ?
C11 C10 C12 110.22(18) . . ?
C2 C7 C9 110.28(18) . . ?
C2 C7 C8 112.76(18) . . ?
C9 C7 C8 111.20(18) . . ?
C4 C5 C6 122.0(2) . . ?
C36 C37 C32 120.4(2) . . ?
C23 C24 C19 121.6(2) . . ?
C21 C20 C19 121.2(2) . . ?
C4 C3 C2 121.3(2) . . ?
C28 C27 C26 120.5(2) . . ?
C15 C14 C13 121.3(2) . . ?
C17 C18 C13 121.3(2) . . ?
C3 C4 C5 119.4(2) . . ?
C16 C17 C18 120.1(2) . . ?
C22 C23 C24 120.3(2) . . ?
C35 C34 C33 120.5(2) . . ?
C16 C15 C14 120.2(2) . . ?
C17 C16 C15 119.9(2) . . ?
C36 C35 C34 119.4(2) . . ?
C23 C22 C21 119.5(2) . . ?
C22 C21 C20 120.4(2) . . ?
C28 C29 C30 119.4(2) . . ?
C29 C28 C27 120.3(2) . . ?
C26 C31 C30 119.5(2) . . ?
C35 C36 C37 120.8(2) . . ?
C29 C30 C31 121.1(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge1 N1 1.9251(17) . ?
Ge1 Cl1 2.3403(8) . ?
Ge1 P1 2.4546(8) . ?
P1 C32 1.812(2) . ?
P1 C26 1.814(2) . ?
P1 C25 1.814(2) . ?
Si1 N1 1.7246(17) . ?
Si1 C19 1.882(2) . ?
Si1 C13 1.893(2) . ?
Si1 C25 1.904(2) . ?
N1 C1 1.443(2) . ?
C1 C6 1.411(3) . ?
C1 C2 1.422(3) . ?
C32 C37 1.388(3) . ?
C32 C33 1.396(3) . ?
C6 C5 1.392(3) . ?
C6 C10 1.527(3) . ?
C13 C14 1.405(3) . ?
C13 C18 1.406(3) . ?
C19 C20 1.399(3) . ?
C19 C24 1.409(3) . ?
C26 C31 1.380(3) . ?
C26 C27 1.398(3) . ?
C2 C3 1.393(3) . ?
C2 C7 1.520(3) . ?
C33 C34 1.389(3) . ?
C10 C11 1.534(3) . ?
C10 C12 1.534(3) . ?
C7 C9 1.534(3) . ?
C7 C8 1.541(3) . ?
C5 C4 1.386(3) . ?
C37 C36 1.381(3) . ?
C24 C23 1.390(3) . ?
C20 C21 1.397(3) . ?
C3 C4 1.379(3) . ?
C27 C28 1.386(3) . ?
C14 C15 1.389(3) . ?
C18 C17 1.395(3) . ?
C17 C16 1.380(4) . ?
C23 C22 1.376(4) . ?
C34 C35 1.379(4) . ?
C15 C16 1.387(4) . ?
C35 C36 1.377(4) . ?
C22 C21 1.389(4) . ?
C29 C28 1.374(4) . ?
C29 C30 1.378(4) . ?
C31 C30 1.394(3) . ?
