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_7707901
_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         'C37 H54 Li N O3 Si'
_chemical_formula_sum            'C37 H54 Li N O3 Si'
_chemical_formula_weight         595.84
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2021-06-02
_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                87.900(2)
_cell_angle_beta                 86.203(2)
_cell_angle_gamma                76.965(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0915(5)
_cell_length_b                   10.2440(5)
_cell_length_c                   17.2833(9)
_cell_measurement_reflns_used    9573
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.41
_cell_measurement_theta_min      2.36
_cell_volume                     1736.41(15)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0344
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            101241
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.474
_diffrn_reflns_theta_min         2.041
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1204 before and 0.0512 after correction. The Ratio of minimum to maximum transmission is 0.9749. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Flack x determined using 7718 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         18604
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0533P)^2^+0.3645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    0.951
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                17307
_reflns_number_total             18604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           lil2
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_database_code               7707901
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.959
_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(C4) = Uanis(C3) = Uanis(C0AA) = Uanis(C5)
3. Others
 Fixed Sof: C025(0.7) H02C(0.7) H02D(0.7) C029(0.7) H02I(0.7) H02J(0.7)
 C02A(0.7) H02K(0.7) H02L(0.7) C02B(0.7) H02M(0.7) H02N(0.7) C0AA(0.3)
 H0AA(0.3) H0AB(0.3) C3(0.3) H3A(0.3) H3B(0.3) C4(0.3) H4A(0.3) H4B(0.3)
 C5(0.3) H5A(0.3) H5B(0.3)
4.a Ternary CH refined with riding coordinates:
 C00R(H00R), C013(H013), C018(H018), C01I(H01I)
4.b Secondary CH2 refined with riding coordinates:
 C00G(H00F,H00G), C00U(H00H,H00J), C00Y(H00D,H00E), C015(H1,HB), C019(H3,HE),
 C01B(H5,HF), C01F(H7,HG), C01N(H01K,H01L), C01O(H01M,H01N), C01Q(H11,HJ),
 C01R(H12,HK), C01S(H01R,H01S), C01V(H14,HL), C01X(H16,HO), C01Z(H17,HP),
 C020(H02Q,H02R), C022(H02A,H02B), C025(H02C,H02D), C026(H02E,H02F), C028(H02G,
 H02H), C029(H02I,H02J), C02A(H02K,H02L), C02B(H02M,H02N), C02C(H02O,H02P),
 C0AA(H0AA,H0AB), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
4.c Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O),
 C00Q(H00Q), C00W(H00W), C00X(H00X), C00Z(H00Z), C011(H011), C012(H012),
 C016(H016), C01A(H4), C01C(H6), C01D(H01D), C01E(H01E), C01G(H01G), C01H(H8),
 C01K(H10), C01T(H13), C01Y(H01Y), C021(H021), C023(H023), C024(H024),
 C027(H027)
4.d Idealised Me refined as rotating group:
 C00T(H00A,H00B,H00C), C010(H01W,H01X,H01Z), C014(H01,H,HA), C017(H2,HC,HD),
 C01J(H9,HH,HI), C01L(H01A,H01B,H01C), C01M(H01F,H01H,H01J), C01P(H01O,H01P,
 H01Q), C01U(H01T,H01U,H01V), C01W(H15,HM,HN)
;
_shelx_res_checksum              33568
_shelx_hkl_checksum              87885
_olex2_submission_special_instructions 'No special instructions were received'