Quasilinear 3d-metal(i) complexes [KM(N(Dipp)SiR<sub>3</sub>)<sub>2</sub>] (M = Cr-Co) - structural diversity, solution state behaviour and reactivity.
Weller, Ruth; Müller, Igor; Duhayon, Carine; Sabo-Etienne, Sylviane; Bontemps, Sébastien; Werncke, C. Gunnar; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4890–4903; doi:10.1039/d1dt00121c

data_7706922
_publ_section_title
;
 Quasilinear 3d-metal(i) complexes
 [KM(N(Dipp)SiR<sub>3</sub>)<sub>2</sub>] (M = Cr-Co) - structural
 diversity, solution state behaviour and reactivity.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4890
_journal_page_last               4903
_journal_paper_doi               10.1039/d1dt00121c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C30 H52 Fe N2 Si2, C16 H32 Li O8'
_chemical_formula_sum            'C46 H84 Fe Li N2 O8 Si2'
_chemical_formula_weight         912.12
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                70.550(2)
_cell_angle_beta                 83.481(2)
_cell_angle_gamma                77.315(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6888(8)
_cell_length_b                   14.5127(10)
_cell_length_c                   16.4126(12)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.30
_cell_volume                     2558.7(3)
_computing_cell_refinement       '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 0.894
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50692
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.504
_diffrn_reflns_theta_min         2.173
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0838 before and 0.0538 after correction. The Ratio of minimum to maximum transmission is 0.9011. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       block
_exptl_crystal_F_000             990
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.242
_refine_diff_density_max         1.456
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         14042
_refine_ls_number_restraints     471
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0826
_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^)+(0.0449P)^2^+14.6421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.1996
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12072
_reflns_number_total             14042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           6_li_12c4_fe
_cod_depositor_comments
'Adding full bibliography for 7706910--7706927.cif.'
_cod_database_code               7706922
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.861
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9137(9)
 0.0863(9)
2. 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
3. Uiso/Uaniso restraints and constraints
C00F \\sim N00C \\sim Si02 \\sim Fe01 \\sim N00D \\sim Si03 \\sim C00E: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O004 \\sim O005 \\sim O009 \\sim O00A \\sim C00M \\sim H00L \\sim H00M \\sim
C00N \\sim H00O \\sim C00P \\sim H00S \\sim H00T \\sim C00Q \\sim H00U \\sim
H00V \\sim C00U \\sim H00Y \\sim H \\sim C00X \\sim H00 \\sim C00Y \\sim H2AA
\\sim HC \\sim C013 \\sim H5AA \\sim HE: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C00F) \\sim Ueq, Uanis(N00C) \\sim Ueq, Uanis(Si02) \\sim Ueq,
Uanis(Fe01) \\sim Ueq, Uanis(N00D) \\sim Ueq, Uanis(Si03) \\sim Ueq,
Uanis(C00E) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O004) \\sim Ueq, Uanis(O005) \\sim Ueq, Uanis(O009) \\sim Ueq,
Uanis(O00A) \\sim Ueq, Uanis(C00M) \\sim Ueq, Uanis(C00N) \\sim Ueq,
Uanis(C00P) \\sim Ueq, Uanis(C00Q) \\sim Ueq, Uanis(C00U) \\sim Ueq,
Uanis(C00X) \\sim Ueq, Uanis(C00Y) \\sim Ueq, Uanis(C013) \\sim Ueq, : with
sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 C00F, N00C, Si02, Fe01, N00D, Si03, C00E
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O004, O005, O009, O00A, C00M, H00L, H00M, C00N, H00O, C00P, H00S, H00T, C00Q,
 H00U, H00V, C00U, H00Y, H, C00X, H00, C00Y, H2AA, HC, C013, H5AA, HE
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C00R(H00R), C018(H018), C01B(H01J), C01E(H01O)
5.b Secondary CH2 refined with riding coordinates:
 C00I(H00J,H00K), C00M(H00L,H00M), C00N(H00N,H00O), C00O(H00P,H00Q), C00P(H00S,
 H00T), C00Q(H00U,H00V), C00T(H00W,H00X), C00U(H00Y,H), C00V(H00Z,HA), C00X(H00,
 HB), C00Y(H2AA,HC), C010(H4AA,HD), C013(H5AA,HE), C014(H6AA,HF), C01F(H7AA,HG)
5.c Aromatic/amide H refined with riding coordinates:
 C011(H011), C015(H015), C016(H016), C019(H019), C01C(H01K), C01G(H01P)
5.d Idealised Me refined as rotating group:
 C00G(H00A,H00B,H00C), C00J(H00D,H00E,H00F), C00W(H00G,H00H,H00I), C012(H01A,
 H01B,H01C), C017(H01D,H01E,H01F), C01A(H01G,H01H,H01I), C01D(H01L,H01M,H01N),
 C01H(H01Q,H01R,H01S), C01I(H01T,H01U,H01V), C01J(H01W,H01X,H01Y), C01K(H01Z,HH,
 HI), C01L(H01,HJ,HK), C01M(H0AA,HL,HM), C01N(H1AA,HN,HO)
;
_shelx_res_checksum              90947
_shelx_hkl_checksum              50601
_olex2_submission_special_instructions 'No special instructions were received'