Homoleptic quasilinear metal(i/ii) silylamides of Cr-Co with phenyl and allyl functions - impact of the oxidation state on secondary ligand interactions.
Weller, Ruth; Ruppach, Lutz; Shlyaykher, Alena; Tambornino, Frank; Werncke, C. Gunnar; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10947–10963; doi:10.1039/d1dt01543e

data_7707910
_publ_section_title
;
 Homoleptic quasilinear metal(i/ii) silylamides of Cr-Co with phenyl and
 allyl functions - impact of the oxidation state on secondary ligand
 interactions.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10947
_journal_page_last               10963
_journal_paper_doi               10.1039/d1dt01543e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C50 H60 Cr0.826 Li0.349 N2 Si2'
_chemical_formula_sum            'C50 H60 Cr0.82 Li0.35 N2 Si2'
_chemical_formula_weight         790.51
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-02 deposited with the CCDC.	2021-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                84.911(8)
_cell_angle_beta                 88.653(8)
_cell_angle_gamma                68.582(7)
_cell_formula_units_Z            2
_cell_length_a                   11.8650(11)
_cell_length_b                   12.9730(13)
_cell_length_c                   16.4026(16)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.771
_cell_measurement_theta_min      2.493
_cell_volume                     2341.0(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'imaging plate area detector'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20595
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.771
_diffrn_reflns_theta_min         2.493
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm LF focus'
_diffrn_source_target            Mo
_diffrn_source_type              'STOE C-Tech Mo LFF X-Ray Tube'
_exptl_absorpt_coefficient_mu    0.291
_exptl_absorpt_correction_T_max  0.9762
_exptl_absorpt_correction_T_min  0.9379
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
X-Area X-Red32 1.63.4.0 (STOE, 2017) Statistics over combined scale factors for x file reflections:
       min. = 0.948 (run 2)   max. = 1.047 (run 2)    spread = 0.1
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       block
_exptl_crystal_F_000             846
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.121
_exptl_crystal_size_rad          0.939
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.0024(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         9847
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0455P)^2^+0.0851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7469
_reflns_number_total             9847
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           crl2
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_database_code               7707910
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.935
_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. Restrained distances
 Si1-N1 \\sim Si1A-N1
 with sigma of 0.02
 Si1-C00G \\sim Si1A-C0AA
 with sigma of 0.02
 Si1-C1 \\sim Si1A-C1A
 with sigma of 0.02
 Si1-C01D \\sim Si1A-C6AA
 with sigma of 0.02
 C00G-C00K \\sim C0AA-C1AA
 with sigma of 0.02
 C00G-C00Y \\sim C0AA-C4AA
 with sigma of 0.02
 C00K-C00U \\sim C1AA-C3AA
 with sigma of 0.02
 C00T-C1 \\sim C2AA-C1A
 with sigma of 0.02
 C00T-C01E \\sim C2AA-C7AA
 with sigma of 0.02
 C00U-C013 \\sim C3AA-C0
 with sigma of 0.02
 C00Y-C014 \\sim C4AA-C3
 with sigma of 0.02
 C1-C01A \\sim C1A-C5AA
 with sigma of 0.02
 C013-C014 \\sim C0-C3
 with sigma of 0.02
 C01A-C01H \\sim C5AA-C9AA
 with sigma of 0.02
 C01E-C01F \\sim C7AA-C8AA
 with sigma of 0.02
 C01F-C01H \\sim C8AA-C9AA
 with sigma of 0.02
 Si1-C00K \\sim Si1A-C1AA
 with sigma of 0.04
 Si1-C00T \\sim Si1A-C2AA
 with sigma of 0.04
 Si1-C00Y \\sim Si1A-C4AA
 with sigma of 0.04
 Si1-C01A \\sim Si1A-C5AA
 with sigma of 0.04
 N1-C00G \\sim N1-C0AA
 with sigma of 0.04
 N1-C1 \\sim N1-C1A
 with sigma of 0.04
 N1-C01D \\sim N1-C6AA
 with sigma of 0.04
 C00G-C00U \\sim C0AA-C3AA
 with sigma of 0.04
 C00G-C1 \\sim C0AA-C1A
 with sigma of 0.04
 C00G-C014 \\sim C0AA-C3
 with sigma of 0.04
 C00G-C01D \\sim C0AA-C6AA
 with sigma of 0.04
 C00K-C00Y \\sim C1AA-C4AA
 with sigma of 0.04
 C00K-C013 \\sim C1AA-C0
 with sigma of 0.04
 C00T-C01A \\sim C2AA-C5AA
 with sigma of 0.04
 C00T-C01F \\sim C2AA-C8AA
 with sigma of 0.04
 C00U-C014 \\sim C3AA-C3
 with sigma of 0.04
 C00Y-C013 \\sim C4AA-C0
 with sigma of 0.04
 C1-C01D \\sim C1A-C6AA
 with sigma of 0.04
 C1-C01E \\sim C1A-C7AA
 with sigma of 0.04
 C1-C01H \\sim C1A-C9AA
 with sigma of 0.04
 C01A-C01F \\sim C5AA-C8AA
 with sigma of 0.04
 C01E-C01H \\sim C7AA-C9AA
 with sigma of 0.04
 C2-C00N \\sim C9-C8
 with sigma of 0.02
 C2-C00P \\sim C9-C7
 with sigma of 0.02
 C00D-C00R \\sim C5-C6
 with sigma of 0.02
 C00D-C010 \\sim C5-C4
 with sigma of 0.02
 C00D-C00N \\sim C5-C8
 with sigma of 0.04
 C00N-C00P \\sim C8-C7
 with sigma of 0.04
 C00R-C010 \\sim C6-C4
 with sigma of 0.04
 C00P-C00R \\sim C7-C6
 with sigma of 0.02
 C00D-C00P \\sim C5-C7
 with sigma of 0.04
 C00N-C010 \\sim C8-C4
 with sigma of 0.02
 Si2-C00N \\sim Si2-C8
 with sigma of 0.04
 Si2-C00P \\sim Si2-C7
 with sigma of 0.04
 C2-C00R \\sim C9-C6
 with sigma of 0.04
 C2-C010 \\sim C9-C4
 with sigma of 0.04
 Si2-C2 \\sim Si2-C9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C0AA) = Uanis(C4AA) = Uanis(C3) = Uanis(C0) = Uanis(C3AA) = Uanis(C1AA)
Uanis(C2AA) = Uanis(C1A) = Uanis(C5AA) = Uanis(C9AA) = Uanis(C8AA) = Uanis(C7AA)
Uanis(C8) = Uanis(C9) = Uanis(C7) = Uanis(C6) = Uanis(C5) = Uanis(C4)
4. Others
 Sof(Si1A)=Sof(C0AA)=Sof(C1AA)=Sof(H1AA)=Sof(C2AA)=Sof(H2AA)=Sof(C3AA)=
 Sof(H3AA)=Sof(C4AA)=Sof(H4AA)=Sof(C1A)=Sof(C0)=Sof(H0)=Sof(C3)=Sof(H3)=
 Sof(C5AA)=Sof(H5AA)=Sof(C6AA)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7AA)=
 Sof(H7AA)=Sof(C8AA)=Sof(H8AA)=Sof(C9AA)=Sof(H9AA)=Sof(Li1)=Sof(Li2)=Sof(C8)=
 Sof(H8)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=
 Sof(C9)=1-FVAR(1)
 Sof(Cr1)=Sof(Si1)=Sof(C2)=Sof(C00D)=Sof(H00D)=Sof(C00G)=Sof(C00K)=Sof(H00K)=
 Sof(C00N)=Sof(H00N)=Sof(C00P)=Sof(H00P)=Sof(C00R)=Sof(H00R)=Sof(C00T)=
 Sof(H00T)=Sof(C00U)=Sof(H00U)=Sof(C00Y)=Sof(H00Y)=Sof(C010)=Sof(H010)=Sof(C1)=
 Sof(C013)=Sof(H013)=Sof(C014)=Sof(H014)=Sof(C01A)=Sof(H01J)=Sof(C01D)=
 Sof(H01Q)=Sof(H01R)=Sof(H01S)=Sof(C01E)=Sof(H01T)=Sof(C01F)=Sof(H01U)=
 Sof(C01H)=Sof(H01Y)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C00B(H00B), C00L(H00L), C00Q(H00Q), C019(H019)
5.b Aromatic/amide H refined with riding coordinates:
 C009(H009), C00D(H00D), C00E(H00E), C00F(H00F), C00J(H00J), C00K(H00K),
 C00M(H00M), C00N(H00N), C00P(H00P), C00R(H00R), C00S(H00S), C00T(H00T),
 C00U(H00U), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010),
 C012(H012), C013(H013), C014(H014), C015(H015), C01A(H01J), C01E(H01T),
 C01F(H01U), C01H(H01Y), C1AA(H1AA), C2AA(H2AA), C3AA(H3AA), C4AA(H4AA), C0(H0),
  C3(H3), C5AA(H5AA), C7AA(H7AA), C8AA(H8AA), C9AA(H9AA), C8(H8), C4(H4),
 C5(H5), C6(H6), C7(H7)
5.c Idealised Me refined as rotating group:
 C00I(H00A,H00C,H00G), C016(H01A,H01B,H01C), C017(H01D,H01E,H01F), C018(H01G,
 H01H,H01I), C01B(H01K,H01L,H01M), C01C(H01N,H01O,H01P), C01D(H01Q,H01R,H01S),
 C01G(H01V,H01W,H01X), C01I(H01Z,H,HA), C01J(H01,HB,HC), C6AA(H6AA,H6AB,H6AC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              97799
_shelx_hkl_checksum              58674
_shelx_fab_checksum              88240
_olex2_submission_special_instructions 'No special instructions were received'