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_7707912
_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
'C46 H73 Co N3 Si2, C20 H40 K O8, 0.7(O1), C4 H8 O0.3'
_chemical_formula_sum            'C70 H121 Co K N3 O9 Si2'
_chemical_formula_weight         1302.90
_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             2021-06-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-12 deposited with the CCDC.	2021-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                102.682(2)
_cell_angle_beta                 100.886(2)
_cell_angle_gamma                94.621(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0565(5)
_cell_length_b                   15.5862(7)
_cell_length_c                   19.4665(8)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.811
_cell_measurement_theta_min      1.933
_cell_volume                     3764.4(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.03
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            77935
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.811
_diffrn_reflns_theta_min         1.933
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.367
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1548 before and 0.0477 after correction. The Ratio of minimum to maximum transmission is 0.9528. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.149
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.203
_exptl_crystal_size_rad          0.062
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         19892
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+4.1222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1374
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14601
_reflns_number_total             19892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           k18c6_col4_ndipp
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_database_code               7707912
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.880
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{O1, C8}
3. Restrained distances
 K1-O00Y \\sim K1-O00Z
 with sigma of 0.02
 O00Y-C024 \\sim O00Z-C3AA
 with sigma of 0.02
 O00Y-C027 \\sim O00Z-C0
 with sigma of 0.02
 C021-C024 \\sim C5AA-C3AA
 with sigma of 0.02
 C021-C02A \\sim C5AA-C0AA
 with sigma of 0.02
 C027-C02A \\sim C0-C0AA
 with sigma of 0.02
 K1-C024 \\sim K1-C3AA
 with sigma of 0.04
 K1-C027 \\sim K1-C0
 with sigma of 0.04
 O00Y-C021 \\sim O00Z-C5AA
 with sigma of 0.04
 O00Y-C02A \\sim O00Z-C0AA
 with sigma of 0.04
 C021-C027 \\sim C5AA-C0
 with sigma of 0.04
 C024-C027 \\sim C3AA-C0
 with sigma of 0.04
 C024-C02A \\sim C3AA-C0AA
 with sigma of 0.04
 K1-O00P \\sim K1-O00Q
 with sigma of 0.02
 O00P-C022 \\sim O00Q-C7AA
 with sigma of 0.02
 O00P-C026 \\sim O00Q-C6AA
 with sigma of 0.02
 C022-C029 \\sim C7AA-C8AA
 with sigma of 0.02
 C026-C02B \\sim C6AA-C1AA
 with sigma of 0.02
 C029-C02B \\sim C8AA-C1AA
 with sigma of 0.02
 K1-C022 \\sim K1-C7AA
 with sigma of 0.04
 K1-C026 \\sim K1-C6AA
 with sigma of 0.04
 O00P-C029 \\sim O00Q-C8AA
 with sigma of 0.04
 O00P-C02B \\sim O00Q-C1AA
 with sigma of 0.04
 C022-C026 \\sim C7AA-C6AA
 with sigma of 0.04
 C022-C02B \\sim C7AA-C1AA
 with sigma of 0.04
 C026-C029 \\sim C6AA-C8AA
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
Uanis(C7AA) = Uanis(C8AA) = Uanis(C1AA) = Uanis(C6AA)
Uanis(C029) = Uanis(C022) = Uanis(C02B) = Uanis(C026)
Uiso(O1) = Uiso(C8)
Uanis(C5AA) = Uanis(C3AA) = Uanis(C0) = Uanis(C0AA)
Uanis(C3BA) = Uanis(C4BA) = Uanis(C44)
Uanis(C15) = Uanis(C10)
5. Others
 Fixed Sof: O00P(0.5) O00Y(0.5) H1BC(0.7) H1BD(0.7) H1AA(0.3) H1AB(0.3)
 C4(0.7) H4A(0.7) H4B(0.7) C5(0.7) H5(0.7) H6BC(0.7) H6BD(0.7) H6AA(0.3)
 H6AB(0.3) C2(0.7) H2A(0.7) C021(0.5) H02A(0.5) H02B(0.5) C022(0.5) H02C(0.5)
 H02D(0.5) C3(0.7) H3A(0.7) H3B(0.7) C024(0.5) H02E(0.5) H02F(0.5) C026(0.5)
 H02G(0.5) H02H(0.5) C027(0.5) H02I(0.5) H02J(0.5) C029(0.5) H02K(0.5)
 H02L(0.5) C02A(0.5) H02M(0.5) H02N(0.5) C02B(0.5) H02O(0.5) H02P(0.5)
 C2AA(0.3) H2AA(0.3) C4AA(0.3) H4AA(0.3) H4AB(0.3) C10(0.3) H10(0.3) C15(0.3)
 H15A(0.3) H15B(0.3) O00Z(0.5) C0(0.5) H0A(0.5) H0B(0.5) C3AA(0.5) H3AA(0.5)
 H3AB(0.5) C0AA(0.5) H0AA(0.5) H0AB(0.5) C5AA(0.5) H5AA(0.5) H5AB(0.5)
 C6AA(0.5) H6AC(0.5) H6AD(0.5) O00Q(0.5) C7AA(0.5) H7AA(0.5) H7AB(0.5)
 C8AA(0.5) H8AA(0.5) H8AB(0.5) C1AA(0.5) H1AC(0.5) H1AD(0.5) O1(0.7) C1BA(0.7)
 H1BA(0.7) H1BB(0.7) C2BA(0.7) H2BA(0.7) H2BB(0.7) C9AA(0.7) H9AA(0.7)
 H9AB(0.7) C0BA(0.7) H0BA(0.7) H0BB(0.7) O5(0.3) C3BA(0.3) H3BA(0.3) H3BB(0.3)
 C4BA(0.3) H4BA(0.3) H4BB(0.3) C8(0.3) H8A(0.3) H8B(0.3) C44(0.3) H44A(0.3)
 H44B(0.3)
6.a Ternary CH refined with riding coordinates:
 C00Q(H00Q), C00T(H00T), C00U(H00U), C013(H013)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1BC,H1BD), C1(H1AA,H1AB), C4(H4A,H4B), C01F(H4,H), C01I(H6,HB), C01J(H7,
 HC), C01K(H8,HD), C01M(H9,HG), C01N(H11,HH), C01O(H12,HI), C01Q(H13,HJ),
 C01R(H14,HK), C01S(H15,HL), C01U(H16,HM), C01X(H17,HR), C021(H02A,H02B),
 C022(H02C,H02D), C024(H02E,H02F), C026(H02G,H02H), C027(H02I,H02J), C029(H02K,
 H02L), C02A(H02M,H02N), C02B(H02O,H02P), C15(H15A,H15B), C0(H0A,H0B),
 C3AA(H3AA,H3AB), C0AA(H0AA,H0AB), C5AA(H5AA,H5AB), C6AA(H6AC,H6AD), C7AA(H7AA,
 H7AB), C8AA(H8AA,H8AB), C1AA(H1AC,H1AD), C1BA(H1BA,H1BB), C2BA(H2BA,H2BB),
 C9AA(H9AA,H9AB), C0BA(H0BA,H0BB), C3BA(H3BA,H3BB), C4BA(H4BA,H4BB), C8(H8A,
 H8B), C44(H44A,H44B)
6.c Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00I(H00I), C00L(H00L), C011(H011), C014(H014), C015(H015),
 C018(H018), C01A(H01M), C01G(H01W), C5(H5), C2(H2A), C2AA(H2AA), C10(H10)
6.d X=CH2 refined with riding coordinates:
 C6(H6BC,H6BD), C6(H6AA,H6AB), C3(H3A,H3B), C4AA(H4AA,H4AB)
6.e Idealised Me refined as rotating group:
 C00W(H00A,H00B,H00C), C00X(H00D,H00E,H00F), C00Z(H00G,H00J,H00M), C010(H01A,
 H01B,H01C), C016(H01D,H01E,H01F), C017(H01G,H01H,H01I), C019(H01J,H01K,H01L),
 C01B(H01N,H01O,H01P), C01C(H01Q,H01R,H01S), C01D(H01T,H01U,H01V), C01H(H01X,
 H01Y,HA), C01L(H01Z,HE,HF), C01V(H01,HN,HO), C01W(H1,HP,HQ), C01Y(H2,HS,HT),
 C01Z(H3,HU,HV)
;
_shelx_res_checksum              54916
_shelx_hkl_checksum              67337
_olex2_submission_special_instructions 'No special instructions were received'