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_7707900
_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'
_chemical_formula_sum            'C60 H64 Fe N2 Si2'
_chemical_formula_weight         925.16
_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             2021-06-12
_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                72.165(2)
_cell_angle_beta                 88.812(2)
_cell_angle_gamma                86.503(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2746(11)
_cell_length_b                   13.7722(10)
_cell_length_c                   17.6349(11)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.168
_cell_measurement_theta_min      2.280
_cell_volume                     2832.6(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99.99
_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 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  0.1147
_diffrn_reflns_av_unetI/netI     0.0766
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66757
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.211
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0958 before and 0.0679 after correction. The Ratio of minimum to maximum transmission is 0.9428. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.104
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         9966
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_gt           0.0584
_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/[\s^2^(Fo^2^)+(0.0727P)^2^+0.1921P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1302
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7076
_reflns_number_total             9966
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           fel3
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_database_code               7707900
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.945
_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. Uiso/Uaniso restraints and constraints
Uanis(C01R) \\sim Ueq, Uanis(C01O) \\sim Ueq, Uanis(C01T) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C01R) = Uanis(C01T)
3.a Ternary CH refined with riding coordinates:
 C00J(H00J), C00Y(H00Y), C01G(H01L), C01O(H01X)
3.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00H(H00H), C00I(H00I), C00K(H00K), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T),
 C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C010(H010), C011(H011),
 C012(H012), C013(H013), C014(H014), C015(H015), C016(H016), C017(H017),
 C018(H018), C01B(H01G), C01C(H01H), C01D(H01I), C01E(H01J), C01F(H01K),
 C01H(H01M), C01J(H01Q), C01K(H01R), C01L(H01S), C01M(H01T), C01Q(H01Z)
3.c Idealised Me refined as rotating group:
 C019(H01A,H01B,H01C), C01A(H01D,H01E,H01F), C01I(H01N,H01O,H01P), C01N(H01U,
 H01V,H01W), C01P(H01Y,H,HA), C01R(H01,HB,HC), C01S(H1,HD,HE), C01T(H2,HF,HG)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38688
_shelx_hkl_checksum              78081
_shelx_fab_checksum              39089
_olex2_submission_special_instructions 'No special instructions were received'