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_7707899
_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         'C38 H48 Li N O2 Si'
_chemical_formula_sum            'C38 H48 Li N O2 Si'
_chemical_formula_weight         585.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-27
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.750(3)
_cell_length_b                   15.312(5)
_cell_length_c                   45.002(11)
_cell_measurement_reflns_used    13263
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.065
_cell_measurement_theta_min      2.276
_cell_volume                     6718(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 (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 0.999
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            97307
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.065
_diffrn_reflns_theta_min         2.276
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1139 before and 0.0518 after correction. The Ratio of minimum to maximum transmission is 0.9415. 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    1.158
_exptl_crystal_description       plate
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 5053 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         13263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0488P)^2^+2.5458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.799
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                12310
_reflns_number_total             13263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01543e2.cif
_cod_data_source_block           lil3_b
_cod_depositor_comments
'Adding full bibliography for 7707896--7707917.cif.'
_cod_original_cell_volume        6719(3)
_cod_database_code               7707899
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.971
_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. Others
 Fixed Sof: H02Q(0.5) H02R(0.5) H02S(0.5) H02T(0.5) H02E(0.5) H02F(0.5)
 H02C(0.5) H02D(0.5) H02Z(0.5) HH(0.5) HI(0.5) HJ(0.5) H02G(0.5) H02H(0.5)
 H02I(0.5) H02J(0.5) C029(0.5) H02K(0.5) H02L(0.5) C02E(0.5) H02M(0.5)
 H02N(0.5) C02F(0.5) H02O(0.5) H02P(0.5) C2AA(0.5) H2AA(0.5) H2AB(0.5)
 C1AA(0.5) H1AB(0.5) H1AC(0.5) C0AA(0.5) H0AB(0.5) H0AC(0.5)
3.a Ternary CH refined with riding coordinates:
 C00R(H00R), C00W(H00W), C00Z(H00Z), C010(H010)
3.b Secondary CH2 refined with riding coordinates:
 C01E(H01F,H01G), C01Q(H01P,H01Q), C01V(H01X,H01Y), C01W(H8AA,HB), C01Z(H0BA,
 HG), C020(H02Q,H02R), C020(H02S,H02T), C021(H02U,H02V), C022(H02A,H02B),
 C024(H02E,H02F), C024(H02C,H02D), C025(H02Z,HH), C025(HI,HJ), C027(H1BA,HM),
 C028(H02G,H02H), C028(H02I,H02J), C029(H02K,H02L), C02A(H2BA,HN), C02E(H02M,
 H02N), C02F(H02O,H02P), C2AA(H2AA,H2AB), C1AA(H1AB,H1AC), C0AA(H0AB,H0AC)
3.c Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00D(H00D), C00E(H00E), C00I(H00I), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
 C00X(H00X), C00Y(H00Y), C012(H012), C014(H014), C015(H015), C018(H018),
 C019(H019), C01A(H0AA), C01B(H01D), C01C(H1AA), C01D(H01E), C01F(H3AA),
 C01G(H01H), C01H(H01I), C01I(H4AA), C01J(H5AA), C01K(H01K), C01L(H01L),
 C01M(H6AA), C01N(H7AA), C01O(H01O), C01R(H01R), C01S(H01S), C01U(H01W)
3.d Idealised Me refined as rotating group:
 C011(H01A,H01B,H01C), C013(H01,H,HA), C01P(H01J,H01M,H01N), C01T(H01T,H01U,
 H01V), C01X(H01Z,HC,HD), C01Y(H9AA,HE,HF), C023(H02W,H02X,H02Y), C026(H02,HK,
 HL)
;
_shelx_res_checksum              75252
_shelx_hkl_checksum              21
_olex2_submission_special_instructions 'No special instructions were received'