#------------------------------------------------------------------------------
#$Date: 2021-06-05 21:01:33 +0300 (Sat, 05 Jun 2021) $
#$Revision: 265933 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/08/1560846.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_1560846
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         'C74 H78 Br6 Ge2 N2 Ni2 P2 Si2'
_chemical_formula_sum            'C74 H78 Br6 Ge2 N2 Ni2 P2 Si2'
_chemical_formula_weight         1855.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                90
_cell_angle_beta                 101.59(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.613(8)
_cell_length_b                   9.870(2)
_cell_length_c                   23.160(5)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      1.92
_cell_volume                     9094(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0897
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_number            8903
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.716
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.795
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       rod
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
The unit cell contains 16 toluene molecules (4 per asymmetric unit) which have been treated
as a diffuse contribution to the overall scattering without specific atom
positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         8903
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0470
_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)+(0.0939P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6105
_reflns_number_total             8903
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1sc00450f2.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
'Adding full bibliography for 1560843--1560857.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1560846
_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+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.58954(2) 0.68830(5) 0.30205(2) 0.02560(14) Uani 1 1 d . . . . .
Br3 Br 0.51383(2) 0.59783(6) 0.32094(3) 0.04359(16) Uani 1 1 d . . . . .
Br2 Br 0.59672(2) 0.92119(5) 0.32427(3) 0.04368(16) Uani 1 1 d . . . . .
Br1 Br 0.59656(2) 0.60222(6) 0.39753(3) 0.04530(17) Uani 1 1 d . . . . .
Ni1 Ni 0.53867(2) 0.65245(6) 0.24114(3) 0.02715(16) Uani 1 1 d . . . . .
P1 P 0.55819(3) 0.72918(13) 0.16697(6) 0.0281(3) Uani 1 1 d . . . . .
Si1 Si 0.63905(3) 0.68659(13) 0.21350(6) 0.0260(3) Uani 1 1 d . . . . .
N1 N 0.62871(9) 0.6317(4) 0.27939(17) 0.0248(8) Uani 1 1 d . . . . .
C1 C 0.64674(11) 0.5194(5) 0.3106(2) 0.0271(10) Uani 1 1 d . . . . .
C13 C 0.67527(11) 0.8104(4) 0.2231(2) 0.0295(11) Uani 1 1 d . . . . .
C2 C 0.67574(12) 0.5447(5) 0.3549(2) 0.0338(11) Uani 1 1 d . . . . .
C26 C 0.55263(12) 0.6145(5) 0.1036(2) 0.0333(11) Uani 1 1 d . . . . .
C25 C 0.60151(11) 0.7891(5) 0.1751(2) 0.0278(10) Uani 1 1 d . . . . .
H25A H 0.602686 0.877289 0.195841 0.033 Uiso 1 1 calc R U . . .
H25B H 0.605122 0.808402 0.134916 0.033 Uiso 1 1 calc R U . . .
C6 C 0.63525(12) 0.3862(5) 0.2971(2) 0.0338(12) Uani 1 1 d . . . . .
C32 C 0.53211(12) 0.8795(5) 0.1434(2) 0.0348(12) Uani 1 1 d . . . . .
C19 C 0.65223(12) 0.5435(5) 0.1702(2) 0.0314(11) Uani 1 1 d . . . . .
C20 C 0.67953(12) 0.4624(5) 0.1944(2) 0.0365(12) Uani 1 1 d . . . . .
H20 H 0.689844 0.475132 0.234635 0.044 Uiso 1 1 calc R U . . .
C18 C 0.70298(12) 0.7874(5) 0.1968(2) 0.0339(11) Uani 1 1 d . . . . .
H18 H 0.704024 0.706859 0.174763 0.041 Uiso 1 1 calc R U . . .
C10 C 0.60370(13) 0.3523(5) 0.2528(3) 0.0372(12) Uani 1 1 d . . . . .
H10 H 0.595945 0.436852 0.230399 0.045 Uiso 1 1 calc R U . . .
C7 C 0.68775(13) 0.6872(6) 0.3737(2) 0.0383(12) Uani 1 1 d . . . . .
H7 H 0.671990 0.753054 0.349591 0.046 Uiso 1 1 calc R U . . .
C5 C 0.65431(15) 0.2794(5) 0.3280(3) 0.0442(14) Uani 1 1 d . . . . .
H5 H 0.647062 0.188488 0.320152 0.053 Uiso 1 1 calc R U . . .
C21 C 0.69232(14) 0.3643(6) 0.1626(3) 0.0421(13) Uani 1 1 d . . . . .
H21 H 0.710980 0.310715 0.180727 0.051 Uiso 1 1 calc R U . . .
C16 C 0.72800(13) 0.9998(6) 0.2342(3) 0.0468(14) Uani 1 1 d . . . . .
H16 H 0.745877 1.063385 0.238253 0.056 Uiso 1 1 calc R U . . .
C14 C 0.67492(13) 0.9297(5) 0.2544(3) 0.0388(12) Uani 1 1 d . . . . .
H14 H 0.656508 0.947573 0.272916 0.047 Uiso 1 1 calc R U . . .
C27 C 0.54552(13) 0.4780(6) 0.1094(3) 0.0408(13) Uani 1 1 d . . . . .
H27 H 0.542858 0.444350 0.146645 0.049 Uiso 1 1 calc R U . . .
C17 C 0.72904(13) 0.8815(6) 0.2026(3) 0.0438(14) Uani 1 1 d . . . . .
H17 H 0.747704 0.864218 0.184705 0.053 Uiso 1 1 calc R U . . .
C3 C 0.69381(14) 0.4354(6) 0.3825(3) 0.0464(14) Uani 1 1 d . . . . .
H3 H 0.713827 0.450544 0.410971 0.056 Uiso 1 1 calc R U . . .
C31 C 0.55668(14) 0.6610(6) 0.0487(2) 0.0430(13) Uani 1 1 d . . . . .
H31 H 0.562365 0.753191 0.044005 0.052 Uiso 1 1 calc R U . . .
C24 C 0.63815(13) 0.5220(6) 0.1102(2) 0.0411(13) Uani 1 1 d . . . . .
H24 H 0.619549 0.575436 0.091721 0.049 Uiso 1 1 calc R U . . .
C15 C 0.70085(14) 1.0241(5) 0.2596(3) 0.0465(14) Uani 1 1 d . . . . .
H15 H 0.699710 1.105824 0.280773 0.056 Uiso 1 1 calc R U . . .
C4 C 0.68285(15) 0.3041(6) 0.3689(3) 0.0512(16) Uani 1 1 d . . . . .
H4 H 0.695425 0.230243 0.388274 0.061 Uiso 1 1 calc R U . . .
C30 C 0.55244(15) 0.5728(7) 0.0004(3) 0.0533(16) Uani 1 1 d . . . . .
H30 H 0.554713 0.605362 -0.037173 0.064 Uiso 1 1 calc R U . . .
C9 C 0.68700(16) 0.7116(7) 0.4388(3) 0.0549(16) Uani 1 1 d . . . . .
H9A H 0.664384 0.692987 0.445604 0.082 Uiso 1 1 calc R U . . .
H9B H 0.692956 0.806029 0.448967 0.082 Uiso 1 1 calc R U . . .
H9C H 0.703182 0.651291 0.463408 0.082 Uiso 1 1 calc R U . . .
C11 C 0.57565(15) 0.3082(6) 0.2859(3) 0.0562(17) Uani 1 1 d . . . . .
H11A H 0.581950 0.222201 0.306267 0.084 Uiso 1 1 calc R U . . .
H11B H 0.554441 0.296764 0.257436 0.084 Uiso 1 1 calc R U . . .
H11C H 0.572910 0.377830 0.314684 0.084 Uiso 1 1 calc R U . . .
C29 C 0.54507(15) 0.4404(7) 0.0076(3) 0.0551(16) Uani 1 1 d . . . . .
H29 H 0.541784 0.380847 -0.025279 0.066 Uiso 1 1 calc R U . . .
C22 C 0.67739(16) 0.3450(6) 0.1033(3) 0.0537(16) Uani 1 1 d . . . . .
H22 H 0.685628 0.276942 0.080919 0.064 Uiso 1 1 calc R U . . .
C12 C 0.60885(15) 0.2437(6) 0.2080(3) 0.0514(15) Uani 1 1 d . . . . .
H12A H 0.626660 0.272611 0.187793 0.077 Uiso 1 1 calc R U . . .
H12B H 0.587882 0.231104 0.179068 0.077 Uiso 1 1 calc R U . . .
H12C H 0.615282 0.157986 0.228576 0.077 Uiso 1 1 calc R U . . .
C8 C 0.72304(14) 0.7143(7) 0.3626(3) 0.0509(15) Uani 1 1 d . . . . .
H8A H 0.738973 0.650992 0.385964 0.076 Uiso 1 1 calc R U . . .
H8B H 0.729657 0.807469 0.374219 0.076 Uiso 1 1 calc R U . . .
H8C H 0.723122 0.701888 0.320690 0.076 Uiso 1 1 calc R U . . .
C23 C 0.65090(16) 0.4245(6) 0.0778(3) 0.0539(16) Uani 1 1 d . . . . .
H23 H 0.641121 0.412755 0.037227 0.065 Uiso 1 1 calc R U . . .
C28 C 0.54230(15) 0.3915(6) 0.0625(3) 0.0526(16) Uani 1 1 d . . . . .
H28 H 0.538158 0.297953 0.067591 0.063 Uiso 1 1 calc R U . . .
C37 C 0.53327(17) 0.9862(6) 0.1810(3) 0.0628(19) Uani 1 1 d . . . . .
H37 H 0.549168 0.984286 0.217201 0.075 Uiso 1 1 calc R U . . .
C33 C 0.50863(19) 0.8844(8) 0.0893(3) 0.073(2) Uani 1 1 d . . . . .
H33 H 0.507062 0.810678 0.062461 0.088 Uiso 1 1 calc R U . . .
C36 C 0.51236(19) 1.0965(7) 0.1687(4) 0.079(2) Uani 1 1 d . . . . .
H36 H 0.513031 1.166860 0.196923 0.094 Uiso 1 1 calc R U . . .
C35 C 0.49056(18) 1.1038(8) 0.1154(4) 0.073(2) Uani 1 1 d . . . . .
H35 H 0.477038 1.182171 0.105240 0.087 Uiso 1 1 calc R U . . .
C34 C 0.48827(19) 0.9941(10) 0.0754(3) 0.086(3) Uani 1 1 d . . . . .
H34 H 0.472572 0.997093 0.038970 0.104 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'
Ni Ni 0.3393 1.1124 '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'
Br Br -0.2901 2.4595 '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 Ni1 119.91(12) . . ?
N1 Ge1 Br1 102.10(12) . . ?
Ni1 Ge1 Br1 116.91(4) . . ?
N1 Ge1 Br2 106.19(12) . . ?
Ni1 Ge1 Br2 110.03(3) . . ?
Br1 Ge1 Br2 99.31(3) . . ?
Ni1 Br3 Ni1 86.96(3) . 2_655 ?
P1 Ni1 Ge1 90.35(4) . . ?
P1 Ni1 Br3 172.22(5) . . ?
Ge1 Ni1 Br3 91.60(3) . . ?
P1 Ni1 Br3 91.51(5) . 2_655 ?
Ge1 Ni1 Br3 175.82(3) . 2_655 ?
Br3 Ni1 Br3 87.06(4) . 2_655 ?
C25 P1 C26 104.1(2) . . ?
C25 P1 C32 104.7(2) . . ?
C26 P1 C32 106.8(2) . . ?
C25 P1 Ni1 121.88(16) . . ?
C26 P1 Ni1 114.44(17) . . ?
C32 P1 Ni1 103.70(17) . . ?
N1 Si1 C19 112.2(2) . . ?
N1 Si1 C13 114.6(2) . . ?
C19 Si1 C13 104.6(2) . . ?
N1 Si1 C25 105.24(19) . . ?
C19 Si1 C25 116.2(2) . . ?
C13 Si1 C25 104.1(2) . . ?
C1 N1 Si1 119.3(3) . . ?
C1 N1 Ge1 117.9(3) . . ?
Si1 N1 Ge1 121.5(2) . . ?
C6 C1 C2 121.0(4) . . ?
C6 C1 N1 119.6(4) . . ?
C2 C1 N1 119.4(4) . . ?
C14 C13 C18 117.4(4) . . ?
C14 C13 Si1 121.4(4) . . ?
C18 C13 Si1 121.2(4) . . ?
C3 C2 C1 118.8(5) . . ?
C3 C2 C7 118.5(5) . . ?
C1 C2 C7 122.7(4) . . ?
C27 C26 C31 118.3(5) . . ?
C27 C26 P1 121.0(4) . . ?
C31 C26 P1 120.7(4) . . ?
P1 C25 Si1 122.8(2) . . ?
C1 C6 C5 117.4(5) . . ?
C1 C6 C10 123.8(4) . . ?
C5 C6 C10 118.8(5) . . ?
C37 C32 C33 118.1(5) . . ?
C37 C32 P1 119.3(4) . . ?
C33 C32 P1 122.4(5) . . ?
C20 C19 C24 116.3(5) . . ?
C20 C19 Si1 120.6(4) . . ?
C24 C19 Si1 122.6(4) . . ?
C21 C20 C19 123.0(5) . . ?
C17 C18 C13 120.7(5) . . ?
C6 C10 C12 113.7(4) . . ?
C6 C10 C11 109.5(5) . . ?
C12 C10 C11 110.5(4) . . ?
C2 C7 C8 111.8(5) . . ?
C2 C7 C9 110.9(5) . . ?
C8 C7 C9 109.9(5) . . ?
C4 C5 C6 121.3(5) . . ?
C20 C21 C22 119.0(5) . . ?
C15 C16 C17 119.2(5) . . ?
C13 C14 C15 121.7(5) . . ?
C28 C27 C26 121.1(5) . . ?
C16 C17 C18 120.7(5) . . ?
C4 C3 C2 120.4(5) . . ?
C26 C31 C30 120.4(6) . . ?
C23 C24 C19 121.2(5) . . ?
C16 C15 C14 120.3(5) . . ?
C5 C4 C3 121.0(5) . . ?
C29 C30 C31 119.7(6) . . ?
C30 C29 C28 120.5(6) . . ?
C23 C22 C21 119.7(5) . . ?
C22 C23 C24 120.8(6) . . ?
C27 C28 C29 119.9(6) . . ?
C32 C37 C36 122.6(6) . . ?
C34 C33 C32 120.4(7) . . ?
C35 C36 C37 119.3(7) . . ?
C36 C35 C34 119.7(6) . . ?
C33 C34 C35 119.8(7) . . ?
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 1.859(4) . ?
Ge1 Ni1 2.2828(10) . ?
Ge1 Br1 2.3324(9) . ?
Ge1 Br2 2.3608(8) . ?
Br3 Ni1 2.3395(10) . ?
Br3 Ni1 2.3820(11) 2_655 ?
Ni1 P1 2.1679(14) . ?
P1 C25 1.830(5) . ?
P1 C26 1.832(5) . ?
P1 C32 1.841(5) . ?
Si1 N1 1.748(4) . ?
Si1 C19 1.871(5) . ?
Si1 C13 1.891(5) . ?
Si1 C25 1.896(5) . ?
N1 C1 1.440(6) . ?
C1 C6 1.408(7) . ?
C1 C2 1.421(7) . ?
C13 C14 1.384(7) . ?
C13 C18 1.401(7) . ?
C2 C3 1.387(7) . ?
C2 C7 1.522(7) . ?
C26 C27 1.390(7) . ?
C26 C31 1.391(8) . ?
C6 C5 1.415(7) . ?
C6 C10 1.508(8) . ?
C32 C37 1.362(8) . ?
C32 C33 1.415(9) . ?
C19 C20 1.391(7) . ?
C19 C24 1.408(7) . ?
C20 C21 1.379(7) . ?
C18 C17 1.394(7) . ?
C10 C12 1.535(8) . ?
C10 C11 1.557(8) . ?
C7 C8 1.529(7) . ?
C7 C9 1.534(8) . ?
C5 C4 1.363(9) . ?
C21 C22 1.398(9) . ?
C16 C15 1.371(8) . ?
C16 C17 1.383(8) . ?
C14 C15 1.394(7) . ?
C27 C28 1.367(8) . ?
C3 C4 1.385(9) . ?
C31 C30 1.401(8) . ?
C24 C23 1.384(8) . ?
C30 C29 1.358(9) . ?
C29 C28 1.386(9) . ?
C22 C23 1.367(9) . ?
C37 C36 1.375(9) . ?
C33 C34 1.362(10) . ?
C36 C35 1.370(11) . ?
C35 C34 1.415(11) . ?
