#------------------------------------------------------------------------------
#$Date: 2021-04-05 17:18:23 +0300 (Mon, 05 Apr 2021) $
#$Revision: 263682 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/00/1560038.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_1560038
loop_
_publ_author_name
'Lücke, Marcel-Philip'
'Yao, Shenglai'
'Driess, Matthias'
_publ_section_title
;
 Boosting homogeneous chemoselective hydrogenation of olefins mediated by
 a bis(silylenyl)terphenyl-nickel(0) pre-catalyst
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2909
_journal_page_last               2915
_journal_paper_doi               10.1039/D0SC06471H
_journal_volume                  12
_journal_year                    2021
_chemical_formula_sum            'C48 H58 N4 Si2'
_chemical_formula_weight         747.16
_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           'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_audit_update_record
;
2020-08-25 deposited with the CCDC.	2021-01-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.889(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.0720(15)
_cell_length_b                   9.1667(4)
_cell_length_c                   19.7603(11)
_cell_measurement_reflns_used    2387
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.8060
_cell_measurement_theta_min      3.5320
_cell_volume                     4474.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0793
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16755
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.230
_diffrn_reflns_theta_min         2.092
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_description       rod
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4440
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1185
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0652P)²+3.8092P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1412
_refine_ls_wR_factor_ref         0.1746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2589
_reflns_number_total             4440
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc06471h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 1560037--1560040.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1560038
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.997
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
Si1 Si 0.06967(4) 0.30375(10) 0.09641(5) 0.0412(3) Uani 0.898(3) 1 d . . P A 1
N2 N 0.10302(11) 0.2969(3) 0.01912(13) 0.0465(6) Uani 1 1 d . . . . .
C1 C 0.12157(13) 0.4342(3) 0.02886(16) 0.0428(7) Uani 1 1 d . . . . .
N1 N 0.11146(12) 0.4730(3) 0.09049(13) 0.0477(7) Uani 1 1 d . . . . .
C2 C 0.12180(13) 0.1943(3) 0.16121(16) 0.0445(7) Uani 1 1 d . . . . .
C3 C 0.17619(14) 0.1916(4) 0.15358(18) 0.0538(8) Uani 1 1 d . . . . .
H3 H 0.187497 0.253416 0.120145 0.065 Uiso 1 1 calc R U . . .
C4 C 0.21415(15) 0.1032(4) 0.19241(19) 0.0585(9) Uani 1 1 d . . . . .
H4 H 0.250796 0.105439 0.185828 0.070 Uiso 1 1 calc R U . . .
C5 C 0.19859(16) 0.0111(4) 0.24107(19) 0.0587(9) Uani 1 1 d . . . . .
H5 H 0.224175 -0.052112 0.267341 0.070 Uiso 1 1 calc R U . . .
C6 C 0.14580(15) 0.0125(3) 0.25080(17) 0.0520(8) Uani 1 1 d . . . . .
H6 H 0.135225 -0.050188 0.284438 0.062 Uiso 1 1 calc R U . . .
C7 C 0.10687(14) 0.1037(3) 0.21257(15) 0.0435(7) Uani 1 1 d . . . . .
C8 C 0.05159(14) 0.1032(3) 0.23004(15) 0.0442(7) Uani 1 1 d . . . . .
C9 C 0.02538(14) 0.2337(3) 0.24050(16) 0.0485(8) Uani 1 1 d . . . . .
H9 H 0.042609 0.323948 0.234497 0.058 Uiso 1 1 calc R U . . .
C10 C 0.02531(13) -0.0267(3) 0.24039(16) 0.0462(8) Uani 1 1 d . . . . .
H10 H 0.042413 -0.116962 0.234151 0.055 Uiso 1 1 calc R U . . .
C11 C 0.10299(15) 0.1961(4) -0.03926(18) 0.0612(10) Uani 1 1 d D . . . .
C12 C 0.1593(2) 0.1357(8) -0.0395(4) 0.075(2) Uani 0.743(9) 1 d D U P B 3
H12A H 0.183687 0.215400 -0.046818 0.112 Uiso 0.743(9) 1 calc R U P B 3
H12B H 0.157860 0.063963 -0.076562 0.112 Uiso 0.743(9) 1 calc R U P B 3
H12C H 0.172608 0.088592 0.004681 0.112 Uiso 0.743(9) 1 calc R U P B 3
C13 C 0.0807(3) 0.2697(6) -0.1081(3) 0.0647(17) Uani 0.743(9) 1 d D U P B 3
H13A H 0.047214 0.321993 -0.104221 0.097 Uiso 0.743(9) 1 calc R U P B 3
H13B H 0.073017 0.195350 -0.144065 0.097 Uiso 0.743(9) 1 calc R U P B 3
H13C H 0.107468 0.338746 -0.119835 0.097 Uiso 0.743(9) 1 calc R U P B 3
C14 C 0.0625(2) 0.0740(5) -0.0296(3) 0.0651(18) Uani 0.743(9) 1 d D U P B 3
H14A H 0.073462 0.028419 0.015527 0.098 Uiso 0.743(9) 1 calc R U P B 3
H14B H 0.062130 0.000317 -0.065608 0.098 Uiso 0.743(9) 1 calc R U P B 3
H14C H 0.026176 0.115714 -0.032534 0.098 Uiso 0.743(9) 1 calc R U P B 3
C15 C 0.12126(13) 0.6120(3) 0.12802(16) 0.0494(8) Uani 1 1 d D . . . .
C16 C 0.0899(6) 0.7373(9) 0.0917(4) 0.097(4) Uani 0.75(2) 1 d D . P C 5
H16A H 0.102878 0.757150 0.048530 0.146 Uiso 0.75(2) 1 calc R U P C 5
H16B H 0.095046 0.824133 0.120969 0.146 Uiso 0.75(2) 1 calc R U P C 5
H16C H 0.051352 0.712228 0.081763 0.146 Uiso 0.75(2) 1 calc R U P C 5
C17 C 0.1024(5) 0.5892(6) 0.1963(3) 0.063(2) Uani 0.75(2) 1 d D . P C 5
H17A H 0.063335 0.570869 0.188171 0.094 Uiso 0.75(2) 1 calc R U P C 5
H17B H 0.110355 0.676775 0.224705 0.094 Uiso 0.75(2) 1 calc R U P C 5
H17C H 0.121406 0.505431 0.220029 0.094 Uiso 0.75(2) 1 calc R U P C 5
C18 C 0.1817(3) 0.6423(15) 0.1405(6) 0.095(3) Uani 0.75(2) 1 d D . P C 5
H18A H 0.201283 0.555443 0.160230 0.142 Uiso 0.75(2) 1 calc R U P C 5
H18B H 0.189746 0.724289 0.172411 0.142 Uiso 0.75(2) 1 calc R U P C 5
H18C H 0.193146 0.666584 0.096835 0.142 Uiso 0.75(2) 1 calc R U P C 5
C19 C 0.14389(14) 0.5271(3) -0.02141(16) 0.0449(7) Uani 1 1 d . . . . .
C20 C 0.19833(15) 0.5232(4) -0.02390(19) 0.0577(9) Uani 1 1 d . . . . .
H20 H 0.221688 0.462719 0.007132 0.069 Uiso 1 1 calc R U . . .
C21 C 0.21927(16) 0.6071(5) -0.0715(2) 0.0678(11) Uani 1 1 d . . . . .
H21 H 0.256925 0.603847 -0.072991 0.081 Uiso 1 1 calc R U . . .
C22 C 0.18596(17) 0.6945(4) -0.1165(2) 0.0657(10) Uani 1 1 d . . . . .
H22 H 0.200341 0.751179 -0.149356 0.079 Uiso 1 1 calc R U . . .
C23 C 0.13186(16) 0.6997(4) -0.11380(19) 0.0631(10) Uani 1 1 d . . . . .
H23 H 0.108903 0.761521 -0.144603 0.076 Uiso 1 1 calc R U . . .
C24 C 0.10993(15) 0.6160(4) -0.06673(18) 0.0553(9) Uani 1 1 d . . . . .
H24 H 0.072232 0.619598 -0.065571 0.066 Uiso 1 1 calc R U . . .
Si1B Si 0.0223(3) 0.1140(8) 0.0659(4) 0.036(2) Uiso 0.102(3) 1 d . . P A 2
C12B C 0.1182(12) 0.0463(13) -0.0059(10) 0.125(10) Uani 0.257(9) 1 d D U P B 4
H12D H 0.149992 0.057035 0.030291 0.188 Uiso 0.257(9) 1 calc R U P B 4
H12E H 0.126563 -0.021800 -0.040874 0.188 Uiso 0.257(9) 1 calc R U P B 4
H12F H 0.087784 0.008573 0.014007 0.188 Uiso 0.257(9) 1 calc R U P B 4
C13B C 0.1584(6) 0.213(3) -0.0627(14) 0.123(10) Uani 0.257(9) 1 d D U P B 4
H13D H 0.157018 0.296686 -0.094093 0.185 Uiso 0.257(9) 1 calc R U P B 4
H13E H 0.166719 0.124489 -0.086420 0.185 Uiso 0.257(9) 1 calc R U P B 4
H13F H 0.186610 0.230052 -0.022565 0.185 Uiso 0.257(9) 1 calc R U P B 4
C14B C 0.0602(9) 0.219(3) -0.1028(10) 0.119(10) Uani 0.257(9) 1 d D U P B 4
H14D H 0.024285 0.199622 -0.091607 0.179 Uiso 0.257(9) 1 calc R U P B 4
H14E H 0.066947 0.152563 -0.139220 0.179 Uiso 0.257(9) 1 calc R U P B 4
H14F H 0.061766 0.320160 -0.118615 0.179 Uiso 0.257(9) 1 calc R U P B 4
C16B C 0.0735(8) 0.709(3) 0.1016(16) 0.076(8) Uiso 0.25(2) 1 d D . P C 6
H16D H 0.070767 0.722361 0.051853 0.115 Uiso 0.25(2) 1 calc R U P C 6
H16E H 0.078639 0.804579 0.124332 0.115 Uiso 0.25(2) 1 calc R U P C 6
H16F H 0.040221 0.664349 0.111355 0.115 Uiso 0.25(2) 1 calc R U P C 6
C17B C 0.1277(11) 0.581(3) 0.2044(5) 0.061(6) Uiso 0.25(2) 1 d D . P C 6
H17D H 0.095521 0.529914 0.214128 0.091 Uiso 0.25(2) 1 calc R U P C 6
H17E H 0.132050 0.673112 0.229923 0.091 Uiso 0.25(2) 1 calc R U P C 6
H17F H 0.159753 0.519800 0.218588 0.091 Uiso 0.25(2) 1 calc R U P C 6
C18B C 0.1702(6) 0.699(2) 0.1170(11) 0.055(5) Uiso 0.25(2) 1 d D . P C 6
H18D H 0.202327 0.635827 0.125211 0.082 Uiso 0.25(2) 1 calc R U P C 6
H18E H 0.175347 0.781078 0.149021 0.082 Uiso 0.25(2) 1 calc R U P C 6
H18F H 0.164766 0.735018 0.069726 0.082 Uiso 0.25(2) 1 calc R U P C 6
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'
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
N2 Si1 N1 69.19(11) . . ?
N2 Si1 C2 100.19(13) . . ?
N1 Si1 C2 98.48(13) . . ?
N2 Si1 C1 34.92(11) . . ?
N1 Si1 C1 34.65(11) . . ?
C2 Si1 C1 105.19(13) . . ?
C1 N2 C11 130.6(3) . . ?
C1 N2 Si1 92.5(2) . . ?
C11 N2 Si1 136.1(2) . . ?
N1 C1 N2 105.4(3) . . ?
N1 C1 C19 127.5(3) . . ?
N2 C1 C19 126.9(3) . . ?
N1 C1 Si1 53.52(16) . . ?
N2 C1 Si1 52.55(16) . . ?
C19 C1 Si1 168.6(2) . . ?
C1 N1 C15 130.4(3) . . ?
C1 N1 Si1 91.83(19) . . ?
C15 N1 Si1 136.6(2) . . ?
C3 C2 C7 116.8(3) . . ?
C3 C2 Si1 119.7(2) . . ?
C7 C2 Si1 123.1(2) . . ?
C4 C3 C2 122.9(3) . . ?
C3 C4 C5 119.7(4) . . ?
C6 C5 C4 119.1(3) . . ?
C5 C6 C7 122.0(3) . . ?
C6 C7 C2 119.5(3) . . ?
C6 C7 C8 117.6(3) . . ?
C2 C7 C8 122.8(3) . . ?
C10 C8 C9 117.6(3) . . ?
C10 C8 C7 121.4(3) . . ?
C9 C8 C7 120.9(3) . . ?
C9 C9 C8 121.11(19) 2 . ?
C10 C10 C8 121.25(19) 2 . ?
N2 C11 C12 110.8(4) . . ?
N2 C11 C14B 117.6(12) . . ?
N2 C11 C13 111.6(3) . . ?
C12 C11 C13 110.8(5) . . ?
N2 C11 C12B 104.9(8) . . ?
C14B C11 C12B 124.4(14) . . ?
N2 C11 C14 105.6(3) . . ?
C12 C11 C14 111.6(4) . . ?
C13 C11 C14 106.3(4) . . ?
N2 C11 C13B 106.9(8) . . ?
C14B C11 C13B 106.3(15) . . ?
C12B C11 C13B 92.9(15) . . ?
N1 C15 C16 113.1(4) . . ?
N1 C15 C18B 116.9(8) . . ?
N1 C15 C16B 106.4(13) . . ?
C18B C15 C16B 104.8(12) . . ?
N1 C15 C17B 108.6(9) . . ?
C18B C15 C17B 106.9(11) . . ?
C16B C15 C17B 113.4(14) . . ?
N1 C15 C17 106.1(3) . . ?
C16 C15 C17 108.2(5) . . ?
N1 C15 C18 108.4(4) . . ?
C16 C15 C18 111.3(6) . . ?
C17 C15 C18 109.6(5) . . ?
C20 C19 C24 119.7(3) . . ?
C20 C19 C1 119.9(3) . . ?
C24 C19 C1 120.5(3) . . ?
C19 C20 C21 120.2(3) . . ?
C22 C21 C20 120.4(4) . . ?
C23 C22 C21 119.6(3) . . ?
C22 C23 C24 121.0(3) . . ?
C19 C24 C23 119.1(3) . . ?
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
Si1 N2 1.864(3) . ?
Si1 N1 1.887(3) . ?
Si1 C2 1.944(3) . ?
Si1 C1 2.345(3) . ?
N2 C1 1.344(4) . ?
N2 C11 1.478(4) . ?
C1 N1 1.334(4) . ?
C1 C19 1.489(4) . ?
N1 C15 1.473(4) . ?
C2 C3 1.398(5) . ?
C2 C7 1.411(4) . ?
C3 C4 1.379(5) . ?
C4 C5 1.385(5) . ?
C5 C6 1.370(5) . ?
C6 C7 1.403(5) . ?
C7 C8 1.485(4) . ?
C8 C10 1.393(4) . ?
C8 C9 1.397(4) . ?
C9 C9 1.388(6) 2 ?
C10 C10 1.386(6) 2 ?
C11 C12 1.516(5) . ?
C11 C14B 1.520(8) . ?
C11 C13 1.535(5) . ?
C11 C12B 1.542(8) . ?
C11 C14 1.545(5) . ?
C11 C13B 1.547(8) . ?
C15 C16 1.503(5) . ?
C15 C18B 1.508(8) . ?
C15 C16B 1.513(8) . ?
C15 C17B 1.517(8) . ?
C15 C17 1.518(5) . ?
C15 C18 1.519(5) . ?
C19 C20 1.375(5) . ?
C19 C24 1.389(5) . ?
C20 C21 1.387(5) . ?
C21 C22 1.369(5) . ?
C22 C23 1.367(5) . ?
C23 C24 1.390(5) . ?
