#------------------------------------------------------------------------------
#$Date: 2021-12-03 22:51:50 +0200 (Fri, 03 Dec 2021) $
#$Revision: 271043 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/91/4519177.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_4519177
loop_
_publ_author_name
'Bories, Cassandre C.'
'Barbazanges, Marion'
'Derat, Etienne'
'Petit, Marc'
_publ_section_title
;
 Implication of a Silyl Cobalt Dihydride Complex as a Useful Catalyst for
 the Hydrosilylation of Imines
;
_journal_issue                   22
_journal_name_full               'ACS Catalysis'
_journal_page_first              14262
_journal_page_last               14273
_journal_paper_doi               10.1021/acscatal.1c03886
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C27 H44 Co P3 Si'
_chemical_formula_sum            'C27 H44 Co P3 Si'
_chemical_formula_weight         548.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 115.243(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0544(5)
_cell_length_b                   18.8627(10)
_cell_length_c                   9.4650(5)
_cell_measurement_reflns_used    8531
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      30.97
_cell_measurement_theta_min      2.49
_cell_volume                     1462.16(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19747
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         2.159
_exptl_absorpt_coefficient_mu    0.805
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 3266 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         8657
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0301
_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/[σ²(Fo²)+(0.0342P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0617
_refine_ls_wR_factor_ref         0.0639
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_full    0.928
_reflns_Friedel_fraction_max     0.936
_reflns_number_gt                7774
_reflns_number_total             8657
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs1c03886_si_002.cif
_cod_data_source_block           cas130
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4519177
_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+1/2, -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
Co1 Co 0.49467(3) 0.55624(2) 0.77038(3) 0.01462(7) Uani 1 1 d . . . . .
P1 P 0.61715(8) 0.62383(4) 0.97607(8) 0.02225(13) Uani 1 1 d . . . . .
P2 P 0.50113(8) 0.62251(3) 0.58509(7) 0.02157(13) Uani 1 1 d . . . . .
P3 P 0.23752(7) 0.57002(3) 0.71390(7) 0.02005(13) Uani 1 1 d . . . . .
Si1 Si 0.52744(7) 0.44324(3) 0.71653(7) 0.01273(12) Uani 1 1 d . . . . .
C1 C 0.8208(4) 0.65595(17) 1.0104(4) 0.0352(7) Uani 1 1 d . . . . .
H1A H 0.891094 0.615531 1.016065 0.053 Uiso 1 1 calc R U . . .
H1B H 0.867949 0.682310 1.108974 0.053 Uiso 1 1 calc R U . . .
H1C H 0.812144 0.687189 0.924462 0.053 Uiso 1 1 calc R U . . .
C2 C 0.5272(4) 0.70496(15) 1.0102(4) 0.0377(7) Uani 1 1 d . . . . .
H2A H 0.508243 0.738626 0.925301 0.057 Uiso 1 1 calc R U . . .
H2B H 0.601840 0.726045 1.109773 0.057 Uiso 1 1 calc R U . . .
H2C H 0.423122 0.693761 1.013736 0.057 Uiso 1 1 calc R U . . .
C3 C 0.6674(4) 0.58012(18) 1.1631(3) 0.0388(7) Uani 1 1 d . . . . .
H3A H 0.728019 0.536387 1.168461 0.058 Uiso 1 1 calc R U . . .
H3B H 0.566561 0.568692 1.172774 0.058 Uiso 1 1 calc R U . . .
H3C H 0.734640 0.611822 1.248328 0.058 Uiso 1 1 calc R U . . .
C4 C 0.6868(4) 0.61285(17) 0.5568(4) 0.0356(7) Uani 1 1 d . . . . .
H4A H 0.693095 0.564529 0.521694 0.053 Uiso 1 1 calc R U . . .
H4B H 0.782044 0.622020 0.655639 0.053 Uiso 1 1 calc R U . . .
H4C H 0.685330 0.646805 0.477818 0.053 Uiso 1 1 calc R U . . .
C5 C 0.5003(4) 0.71920(15) 0.6069(4) 0.0365(7) Uani 1 1 d . . . . .
H5A H 0.401789 0.733504 0.618122 0.055 Uiso 1 1 calc R U . . .
H5B H 0.501486 0.742000 0.514367 0.055 Uiso 1 1 calc R U . . .
H5C H 0.597180 0.733701 0.699892 0.055 Uiso 1 1 calc R U . . .
C6 C 0.3464(4) 0.61521(17) 0.3818(3) 0.0349(6) Uani 1 1 d . . . . .
H6A H 0.238360 0.625587 0.377051 0.052 Uiso 1 1 calc R U . . .
H6B H 0.347305 0.566996 0.343601 0.052 Uiso 1 1 calc R U . . .
H6C H 0.371274 0.649146 0.316571 0.052 Uiso 1 1 calc R U . . .
C7 C 0.1744(3) 0.55260(17) 0.8706(3) 0.0320(6) Uani 1 1 d . . . . .
H7A H 0.196504 0.502926 0.903090 0.048 Uiso 1 1 calc R U . . .
H7B H 0.057297 0.562071 0.832659 0.048 Uiso 1 1 calc R U . . .
H7C H 0.235637 0.583502 0.959742 0.048 Uiso 1 1 calc R U . . .
C8 C 0.1490(4) 0.65860(15) 0.6584(4) 0.0329(6) Uani 1 1 d . . . . .
H8A H 0.215080 0.692915 0.738037 0.049 Uiso 1 1 calc R U . . .
H8B H 0.037306 0.658573 0.649942 0.049 Uiso 1 1 calc R U . . .
H8C H 0.147285 0.671723 0.557530 0.049 Uiso 1 1 calc R U . . .
C9 C 0.0846(3) 0.51924(15) 0.5533(3) 0.0295(6) Uani 1 1 d . . . . .
H9A H 0.100358 0.468526 0.577646 0.044 Uiso 1 1 calc R U . . .
H9B H 0.096603 0.528684 0.456935 0.044 Uiso 1 1 calc R U . . .
H9C H -0.024893 0.533323 0.539470 0.044 Uiso 1 1 calc R U . . .
C10 C 0.3521(3) 0.38074(11) 0.6985(2) 0.0146(4) Uani 1 1 d . . . . .
C11 C 0.3009(3) 0.38062(13) 0.8192(3) 0.0187(4) Uani 1 1 d . . . . .
H11 H 0.360305 0.407909 0.910299 0.022 Uiso 1 1 calc R U . . .
C12 C 0.1666(3) 0.34206(13) 0.8100(3) 0.0225(5) Uani 1 1 d . . . . .
H12 H 0.134293 0.343997 0.893120 0.027 Uiso 1 1 calc R U . . .
C13 C 0.0797(3) 0.30080(14) 0.6800(3) 0.0242(5) Uani 1 1 d . . . . .
H13 H -0.013605 0.275038 0.672192 0.029 Uiso 1 1 calc R U . . .
C14 C 0.1304(3) 0.29756(14) 0.5619(3) 0.0260(5) Uani 1 1 d . . . . .
H14 H 0.073002 0.268511 0.473229 0.031 Uiso 1 1 calc R U . . .
C15 C 0.2656(3) 0.33672(13) 0.5717(3) 0.0205(5) Uani 1 1 d . . . . .
H15 H 0.299280 0.333212 0.489671 0.025 Uiso 1 1 calc R U . . .
C16 C 0.7095(3) 0.39404(13) 0.8721(2) 0.0164(4) Uani 1 1 d . . . . .
C17 C 0.7223(3) 0.32050(14) 0.8635(3) 0.0242(5) Uani 1 1 d . . . . .
H17 H 0.640781 0.295692 0.778707 0.029 Uiso 1 1 calc R U . . .
C18 C 0.8516(3) 0.28222(15) 0.9760(3) 0.0311(6) Uani 1 1 d . . . . .
H18 H 0.857805 0.232315 0.966095 0.037 Uiso 1 1 calc R U . . .
C19 C 0.9696(3) 0.31711(17) 1.1008(3) 0.0330(7) Uani 1 1 d . . . . .
H19 H 1.057269 0.291443 1.177779 0.040 Uiso 1 1 calc R U . . .
C20 C 0.9596(3) 0.38883(18) 1.1132(3) 0.0375(7) Uani 1 1 d . . . . .
H20 H 1.039831 0.412893 1.200336 0.045 Uiso 1 1 calc R U . . .
C21 C 0.8333(3) 0.42717(16) 0.9996(3) 0.0277(6) Uani 1 1 d . . . . .
H21 H 0.831210 0.477258 1.009113 0.033 Uiso 1 1 calc R U . . .
C22 C 0.5552(3) 0.42509(12) 0.5312(2) 0.0154(4) Uani 1 1 d . . . . .
C23 C 0.7065(3) 0.40734(13) 0.5327(3) 0.0194(5) Uani 1 1 d . . . . .
H23 H 0.799730 0.403939 0.630018 0.023 Uiso 1 1 calc R U . . .
C24 C 0.7235(3) 0.39464(14) 0.3962(3) 0.0236(5) Uani 1 1 d . . . . .
H24 H 0.828144 0.383775 0.401405 0.028 Uiso 1 1 calc R U . . .
C25 C 0.5897(3) 0.39762(15) 0.2524(3) 0.0254(5) Uani 1 1 d . . . . .
H25 H 0.601241 0.387522 0.159218 0.031 Uiso 1 1 calc R U . . .
C26 C 0.4381(3) 0.41564(15) 0.2465(3) 0.0259(5) Uani 1 1 d . . . . .
H26 H 0.345214 0.418241 0.148709 0.031 Uiso 1 1 calc R U . . .
C27 C 0.4227(3) 0.42985(14) 0.3837(3) 0.0203(5) Uani 1 1 d . . . . .
H27 H 0.318894 0.443231 0.377339 0.024 Uiso 1 1 calc R U . . .
H1 H 0.650(4) 0.5348(17) 0.788(4) 0.039(9) Uiso 1 1 d . . . . .
H2 H 0.494(4) 0.5081(17) 0.873(3) 0.035(9) Uiso 1 1 d . . . . .
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'
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'
Co Co 0.3494 0.9721 '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
P3 Co1 P2 97.32(3) . . ?
P3 Co1 P1 103.44(3) . . ?
P2 Co1 P1 101.80(3) . . ?
P3 Co1 Si1 106.86(3) . . ?
P2 Co1 Si1 108.16(3) . . ?
P1 Co1 Si1 133.59(3) . . ?
C3 P1 C2 98.78(16) . . ?
C3 P1 C1 99.29(15) . . ?
C2 P1 C1 100.52(14) . . ?
C3 P1 Co1 114.89(11) . . ?
C2 P1 Co1 123.34(11) . . ?
C1 P1 Co1 116.06(10) . . ?
C4 P2 C5 99.45(15) . . ?
C4 P2 C6 100.23(15) . . ?
C5 P2 C6 98.87(15) . . ?
C4 P2 Co1 113.90(10) . . ?
C5 P2 Co1 118.52(10) . . ?
C6 P2 Co1 122.01(10) . . ?
C9 P3 C8 98.97(14) . . ?
C9 P3 C7 101.05(13) . . ?
C8 P3 C7 98.42(14) . . ?
C9 P3 Co1 119.59(9) . . ?
C8 P3 Co1 118.18(9) . . ?
C7 P3 Co1 116.82(9) . . ?
C22 Si1 C16 102.25(10) . . ?
C22 Si1 C10 103.63(10) . . ?
C16 Si1 C10 100.26(10) . . ?
C22 Si1 Co1 117.54(7) . . ?
C16 Si1 Co1 116.08(7) . . ?
C10 Si1 Co1 114.74(7) . . ?
C15 C10 C11 116.1(2) . . ?
C15 C10 Si1 125.51(17) . . ?
C11 C10 Si1 118.34(16) . . ?
C12 C11 C10 122.3(2) . . ?
C13 C12 C11 120.1(2) . . ?
C14 C13 C12 119.1(2) . . ?
C13 C14 C15 120.5(2) . . ?
C10 C15 C14 121.8(2) . . ?
C21 C16 C17 116.0(2) . . ?
C21 C16 Si1 123.88(19) . . ?
C17 C16 Si1 120.08(17) . . ?
C16 C17 C18 122.0(2) . . ?
C19 C18 C17 119.8(3) . . ?
C20 C19 C18 119.5(2) . . ?
C19 C20 C21 120.7(3) . . ?
C20 C21 C16 121.8(3) . . ?
C27 C22 C23 116.2(2) . . ?
C27 C22 Si1 120.79(17) . . ?
C23 C22 Si1 122.97(16) . . ?
C24 C23 C22 121.9(2) . . ?
C25 C24 C23 120.7(2) . . ?
C24 C25 C26 118.9(2) . . ?
C27 C26 C25 120.0(2) . . ?
C26 C27 C22 122.2(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
Co1 P3 2.1709(6) . ?
Co1 P2 2.1746(7) . ?
Co1 P1 2.1918(7) . ?
Co1 Si1 2.2406(7) . ?
P1 C3 1.826(3) . ?
P1 C2 1.826(3) . ?
P1 C1 1.833(3) . ?
P2 C4 1.821(3) . ?
P2 C5 1.836(3) . ?
P2 C6 1.839(3) . ?
P3 C9 1.830(3) . ?
P3 C8 1.830(3) . ?
P3 C7 1.832(2) . ?
Si1 C22 1.906(2) . ?
Si1 C16 1.917(2) . ?
Si1 C10 1.925(2) . ?
C10 C15 1.394(3) . ?
C10 C11 1.404(3) . ?
C11 C12 1.388(3) . ?
C12 C13 1.383(4) . ?
C13 C14 1.379(4) . ?
C14 C15 1.399(3) . ?
C16 C21 1.396(3) . ?
C16 C17 1.397(3) . ?
C17 C18 1.401(3) . ?
C18 C19 1.376(4) . ?
C19 C20 1.364(5) . ?
C20 C21 1.392(4) . ?
C22 C27 1.403(3) . ?
C22 C23 1.404(3) . ?
C23 C24 1.385(3) . ?
C24 C25 1.385(4) . ?
C25 C26 1.392(4) . ?
C26 C27 1.390(3) . ?
