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_7707905
_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         'C52 H80 Co K N2 O6 Si2'
_chemical_formula_sum            'C52 H80 Co K N2 O6 Si2'
_chemical_formula_weight         983.39
_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             2021-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-12 deposited with the CCDC.	2021-07-07 downloaded from the CCDC.
;
_cell_angle_alpha                85.095(6)
_cell_angle_beta                 75.862(6)
_cell_angle_gamma                77.123(6)
_cell_formula_units_Z            2
_cell_length_a                   10.688(2)
_cell_length_b                   15.427(3)
_cell_length_c                   17.610(4)
_cell_measurement_reflns_used    5792
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.50
_cell_measurement_theta_min      2.22
_cell_volume                     2743.4(10)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1123
_diffrn_reflns_av_unetI/netI     0.1104
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29137
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.086
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1190 before and 0.0569 after correction. The Ratio of minimum to maximum transmission is 0.8461. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.274
_exptl_crystal_size_min          0.124
_exptl_crystal_size_rad          0.062
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         9518
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0593P)^2^+1.1857P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5679
_reflns_number_total             9518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           k18c6_col1
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_original_cell_volume        2743.5(10)
_cod_database_code               7707905
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.756
_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
Uanis(C0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C0AA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: H017(0.5) H01P(0.5) C01S(0.3) H2BA(0.3) HN(0.3) HO(0.3) C0AA(0.7)
 H0AB(0.7) H0AC(0.7) H0AD(0.7)
5.a Ternary CH refined with riding coordinates:
 C00K(H00K), C00L(H00L), C00U(H00U), C017(H017), C017(H01P)
5.b Secondary CH2 refined with riding coordinates:
 C00Q(H00D,H00E), C00X(H00J,H00M), C00Z(H00N,H00Q), C011(H01D,H01E), C015(H01L,
 H01M), C016(H01N,H01O), C019(H01Q,H01R), C01A(H01S,H01T), C01B(H01U,H01V),
 C01F(H01,HC), C01G(H0AA,HD), C01I(H2AA,HG)
5.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00O(H00O), C00P(H00P), C00S(H00S), C00T(H00T), C00W(H00W),
 C00Y(H00Y), C014(H014), C018(H018), C01C(H01W), C01J(H3AA), C01L(H5AA),
 C01N(H7AA), C01O(H8AA), C01P(H9AA), C01Q(H0BA)
5.d Idealised Me refined as rotating group:
 C00N(H00A,H00B,H00C), C00V(H00F,H00G,H00H), C010(H01A,H01B,H01C), C012(H01F,
 H01G,H01H), C013(H01I,H01J,H01K), C01D(H01X,H01Y,H), C01E(H01Z,HA,HB),
 C01H(H1AA,HE,HF), C01K(H4AA,HH,HI), C01M(H6AA,HJ,HK), C01R(H1BA,HL,HM),
 C01S(H2BA,HN,HO), C0AA(H0AB,H0AC,H0AD)
;
_shelx_res_checksum              99016
_shelx_hkl_checksum              11788
_olex2_submission_special_instructions 'No special instructions were received'