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_7707914
_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
'C60 H64 Fe N2 Si2, 2(C10 H20 K0.5 O4), [+ solvents]1[n-pentane]'
_chemical_formula_sum            'C80 H104 Fe K N2 O8 Si2'
_chemical_formula_weight         1372.78
_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             2021-06-08
_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                79.978(2)
_cell_angle_beta                 88.219(2)
_cell_angle_gamma                73.252(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5267(8)
_cell_length_b                   13.5299(9)
_cell_length_c                   24.9620(15)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.23
_cell_volume                     3988.6(4)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_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  0.0870
_diffrn_reflns_av_unetI/netI     0.1105
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            54903
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.904
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0974 before and 0.0539 after correction. The Ratio of minimum to maximum transmission is 0.9423. 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    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1470
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     903
_refine_ls_number_reflns         14023
_refine_ls_number_restraints     186
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0713
_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^)+(0.0692P)^2^+2.1184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1399
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9138
_reflns_number_total             14023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           k18c6_fel3
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_database_code               7707914
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.920
_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. Restrained distances
 C9-C10 = C11-C12
 1.53 with sigma of 0.02
 O2-C9 = O2-C12
 1.44 with sigma of 0.02
 C10-C11
 1.54 with sigma of 0.02
 C13-C14 = C15-C16
 1.53 with sigma of 0.02
 O1-C13 = O1-C16
 1.44 with sigma of 0.02
 C14-C15
 1.54 with sigma of 0.02
 O2-C10 = O2-C11 = C9-C11 = C10-C12
 2.38 with sigma of 0.04
 O1-C14 = O1-C15 = C13-C15 = C14-C16
 2.38 with sigma of 0.04
 O2-C9 \\sim O2-C12
 with sigma of 0.02
 C9-C10 \\sim C10-C11 \\sim C11-C12
 with sigma of 0.02
 O2-C10 \\sim O2-C11
 with sigma of 0.04
 C10-C12 \\sim C9-C11
 with sigma of 0.04
 C13-C14 \\sim C14-C15 \\sim C15-C16
 with sigma of 0.02
 O1-C14 \\sim O1-C15
 with sigma of 0.04
 C14-C16 \\sim C13-C15
 with sigma of 0.04
 O1-C13 \\sim O1-C16
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O2 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O1 \\sim C13 \\sim C14 \\sim C15 \\sim C16: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(C0BA) \\sim Ueq, Uanis(C00P) \\sim Ueq, Uanis(C00S) \\sim Ueq,
Uanis(C01B) \\sim Ueq, Uanis(C00M) \\sim Ueq, Uanis(C00U) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O2, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C13, C14, C15, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O2(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5) H10A(0.5) H10B(0.5)
 C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5) O1(0.5) C13(0.5)
 H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5) C15(0.5) H15A(0.5) H15B(0.5)
 C16(0.5) H16A(0.5) H16B(0.5)
6.a Ternary CH refined with riding coordinates:
 C013(H013), C01D(H01D), C01R(H01X), C01Y(H3)
6.b Secondary CH2 refined with riding coordinates:
 C01W(H5,HB), C01Z(H4,HE), C021(H02K,H02L), C023(H02U,H02V), C024(H02W,H02X),
 C025(H02Y,HF), C026(H02M,H02N), C027(H02O,H02P), C028(H02Z,HG), C02A(H02,HH),
 C02B(H02Q,H02R), C02C(H6,HI), C02G(H02S,H02T), C02H(H7,HJ), C02I(H8,HK),
 C02K(H9,HL), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
6.c Aromatic/amide H refined with riding coordinates:
 C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
 C00W(H00W), C00X(H00X), C00Y(H00Y), C010(H010), C012(H012), C014(H014),
 C015(H015), C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A),
 C01B(H01B), C01C(H01C), C01F(H01H), C01G(H01I), C01H(H01J), C01I(H01K),
 C01J(H01L), C01K(H01M), C01L(H01N), C01M(H01O), C01N(H01P), C01O(H01Q),
 C01S(H01Y), C01T(H01Z), C01V(H1), C020(H020), C022(H022), C02D(H02D)
6.d Idealised Me refined as rotating group:
 C01E(H01E,H01F,H01G), C01P(H01R,H01S,H01T), C01Q(H01U,H01V,H01W), C01U(H01,H,
 HA), C01X(H2,HC,HD), C029(H02A,H02B,H02C), C02E(H02E,H02F,H02G), C02F(H02H,
 H02I,H02J)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23600
_shelx_hkl_checksum              2991
_shelx_fab_checksum              19603
_olex2_submission_special_instructions 'No special instructions were received'