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_7707916
_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
'0.5(C40 H56 Fe N2 Si2), C28 H45 Fe0.5 K0.5 N O3.5 Si, 0.5(C16 H34 K O7)'
_chemical_formula_sum            'C56 H90 Fe K N2 O7 Si2'
_chemical_formula_weight         1054.42
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-13 deposited with the CCDC.	2021-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                60.863(7)
_cell_angle_beta                 66.609(9)
_cell_angle_gamma                79.327(9)
_cell_formula_units_Z            4
_cell_length_a                   18.141(2)
_cell_length_b                   19.9930(19)
_cell_length_c                   20.561(2)
_cell_measurement_reflns_used    20942
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.447
_cell_volume                     5978.0(12)
_computing_cell_refinement       'X-Area Recipe 1.36.0.0 (STOE, 2020)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction        'X-Area X-Red 1.65.2.0 (STOE, 2020)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_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  0.0650
_diffrn_reflns_av_unetI/netI     0.0742
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41617
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.447
_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    0.410
_exptl_absorpt_correction_T_max  0.9617
_exptl_absorpt_correction_T_min  0.4748
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
X-Area LANA 1.71.6.0 (STOE, 2017) Statistics over combined scale factors for x file reflections:
       min. = 0.782 (run 2)   max. = 1.585 (run 1)    spread = 0.8
;
_exptl_crystal_colour            'clear reddish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       plate
_exptl_crystal_F_000             2276
_exptl_crystal_size_max          0.702
_exptl_crystal_size_mid          0.604
_exptl_crystal_size_min          0.161
_exptl_crystal_size_rad          0.062
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1394
_refine_ls_number_reflns         20923
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1284P)^2^+10.3312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2276
_refine_ls_wR_factor_ref         0.2420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14208
_reflns_number_total             20923
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           k18c6_fel1
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_original_cell_volume        5977.9(13)
_cod_database_code               7707916
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.762
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C7AA \\sim C1BA \\sim C6AA \\sim C3AA \\sim C4AA: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
C2BA \\sim C8AA \\sim C5AA \\sim C9AA \\sim C0BA: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
Uanis(C9) \\sim Ueq, Uanis(C4BA) \\sim Ueq, Uanis(C5BA) \\sim Ueq, Uanis(C3BA)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C9) \\sim Ueq, Uanis(C4BA) \\sim Ueq, Uanis(C3BA) \\sim Ueq, Uanis(C5BA)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C7AA) \\sim Ueq, Uanis(C1BA) \\sim Ueq, Uanis(C6AA) \\sim Ueq,
Uanis(C3AA) \\sim Ueq, Uanis(C4AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C2BA) \\sim Ueq, Uanis(C8AA) \\sim Ueq, Uanis(C5AA) \\sim Ueq,
Uanis(C9AA) \\sim Ueq, Uanis(C0BA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C0CA) = Uanis(C3CA) = Uanis(C2CA) = Uanis(C40)
Uanis(C2CA) = Uanis(C40) = Uanis(C6BA) = Uanis(C7BA) = Uanis(C0CA) =
Uanis(C3CA) = Uanis(C8BA) = Uanis(C9BA)
3. Rigid body (RIGU) restrains
 C7AA, C1BA, C6AA, C3AA, C4AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2BA, C8AA, C5AA, C9AA, C0BA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: H01A(0.5) H01b(0.5) H02H(0.5) H02d(0.5) C3AA(0.5) H3AA(0.5)
 C4AA(0.5) H4AA(0.5) C1BA(0.5) H1BA(0.5) C6AA(0.5) H6AA(0.5) C7AA(0.5)
 H7AA(0.5) C8CA(0.5) H8CA(0.5) C9CA(0.5) H9CA(0.5) C0DA(0.5) H0DA(0.5)
 C1DA(0.5) H1DA(0.5) C5(0.5) H5(0.5) C1AA(0.5) H1AA(0.5) C2AA(0.5) H2AA(0.5)
 C0AA(0.5) H0AA(0.5) C6(0.5) H6(0.5) C8(0.5) H8(0.5) C5AA(0.5) H5AA(0.5)
 C2BA(0.5) H2BA(0.5) C0BA(0.5) H0BA(0.5) C8AA(0.5) H8AA(0.5) C9AA(0.5)
 H9AA(0.5) C4BA(0.5) H4Ba(0.5) H4Bb(0.5) H4Bc(0.5) C3BA(0.5) H3Ba(0.5)
 H3Bb(0.5) H3Bc(0.5) C5BA(0.5) H5Ba(0.5) H5Bb(0.5) H5Bc(0.5) C9(0.5) H9a(0.5)
 H9b(0.5) H9c(0.5) O1(0.5) C7BA(0.7) H7Ba(0.7) H7Bb(0.7) C8BA(0.7) H8Ba(0.7)
 H8Bb(0.7) C6BA(0.7) H6Ba(0.7) H6Bb(0.7) H6Bc(0.7) C9BA(0.7) H9Ba(0.7)
 H9Bb(0.7) H9Bc(0.7) O3CA(0.5) C2CA(0.3) H2Ca(0.3) H2Cb(0.3) C40(0.3) H40a(0.3)
 H40b(0.3) H40c(0.3) C3CA(0.3) H3Ca(0.3) H3Cb(0.3) H3Cc(0.3) C0CA(0.3)
 H0Ca(0.3) H0Cb(0.3) C4CA(0.5) H4Ca(0.5) H4Cb(0.5) H4Cc(0.5) C5CA(0.5)
 H5Ca(0.5) H5Cb(0.5) H5Cc(0.5) C7CA(0.5) H7Ca(0.5) H7Cb(0.5) H7Cc(0.5)
 C6CA(0.5) H6Ca(0.5) H6Cb(0.5) H6Cc(0.5)
5.a Ternary CH refined with riding coordinates:
 C015(H015), C017(H017), C01A(H01A), C01A(H01b), C01D(H01D), C01F(H01l),
 C01W(H1), C027(H027), C02H(H02H), C02H(H02d)
5.b Secondary CH2 refined with riding coordinates:
 C01B(H4,H), C01O(H7,Ha), C01P(H17,Hb), C01U(H18,Hc), C01V(H19,Hd), C023(H9,
 He), C024(H10,Hf), C026(H20,Hg), C02A(H11,Hj), C02B(H12,Hk), C02F(H22,Hl),
 C02K(H24,Ho), C02L(H13,Hp), C02M(H25,Hq), C02N(H26,Hr), C02Q(H14,Hs), C02S(H15,
 Hv), C02U(H27,Hw), C02Z(H16,H29), C030(H03n,H03o), C032(H03r,H03s), C036(H03p,
 H03q), C037(H03t,H03u), C038(H03v,H03w), C039(H03x,H03y), C03D(H03z,H30),
 C7BA(H7Ba,H7Bb), C8BA(H8Ba,H8Bb), C2CA(H2Ca,H2Cb), C0CA(H0Ca,H0Cb)
5.c Aromatic/amide H refined with riding coordinates:
 C00W(H00W), C00Z(H00Z), C010(H010), C013(H013), C016(H016), C019(H019),
 C01G(H01n), C01H(H01H), C01I(H01o), C01T(H01), C01X(H01X), C022(H022),
 C02D(H02o), C3AA(H3AA), C4AA(H4AA), C1BA(H1BA), C6AA(H6AA), C7AA(H7AA),
 C02X(H02), C03C(H03m), C028(H028), C021(H021), C02I(H3), C031(H031),
 C8CA(H8CA), C9CA(H9CA), C0DA(H0DA), C1DA(H1DA), C5(H5), C1AA(H1AA), C2AA(H2AA),
  C0AA(H0AA), C6(H6), C8(H8), C5AA(H5AA), C2BA(H2BA), C0BA(H0BA), C8AA(H8AA),
 C9AA(H9AA)
5.d Fitted hexagon refined as free rotating group:
 C02T(C3AA,C4AA,C1BA,C6AA,C7AA), C03C(C028,C021,C1,C02I,C031)
5.e Idealised Me refined as rotating group:
 C01J(H01c,H01e,H01f), C01L(H01p,H01q,H01r), C01N(H01s,H01t,H01u), C01R(H01v,
 H01w,H01y), C01Y(H01g,H01i,H01j), C020(H02i,H02j,H02k), C025(H02l,H02m,H02n),
 C029(H21,Hh,Hi), C02C(H02a,H02b,H02c), C02E(H02p,H02q,H02r), C1CA(H1Ca,H1Cb,
 H1Cc), C02J(H23,Hm,Hn), C02O(H02s,H02t,H02u), C02P(H02v,H02w,H02x), C02R(H02y,
 Ht,Hu), C02V(H02z,Hx,Hy), C02W(H02e,H02f,H02g), C02Y(H2,Hz,H28), C033(H03a,
 H03b,H03c), C034(H03d,H03e,H03f), C035(H03j,H03k,H03l), C03B(H03g,H03h,H03i),
 C4BA(H4Ba,H4Bb,H4Bc), C3BA(H3Ba,H3Bb,H3Bc), C5BA(H5Ba,H5Bb,H5Bc), C9(H9a,H9b,
 H9c), C6BA(H6Ba,H6Bb,H6Bc), C9BA(H9Ba,H9Bb,H9Bc), C40(H40a,H40b,H40c),
 C3CA(H3Ca,H3Cb,H3Cc), C4CA(H4Ca,H4Cb,H4Cc), C5CA(H5Ca,H5Cb,H5Cc), C7CA(H7Ca,
 H7Cb,H7Cc), C6CA(H6Ca,H6Cb,H6Cc)
;
_shelx_res_checksum              80212
_shelx_hkl_checksum              18965
_olex2_submission_special_instructions 'No special instructions were received'