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_7706918
_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         'C54 H98 Cr K N2 O3 Si2'
_chemical_formula_sum            'C54 H98 Cr K N2 O3 Si2'
_chemical_formula_weight         970.62
_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
_audit_creation_date             2021-02-10
_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                93.330(5)
_cell_angle_beta                 95.457(5)
_cell_angle_gamma                97.740(5)
_cell_formula_units_Z            2
_cell_length_a                   11.886(2)
_cell_length_b                   14.190(2)
_cell_length_c                   17.464(3)
_cell_measurement_reflns_used    9058
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      21.46
_cell_measurement_theta_min      2.42
_cell_volume                     2897.9(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23343
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        14.853
_diffrn_reflns_theta_max         14.853
_diffrn_reflns_theta_min         2.197
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.7438
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1202 before and 0.0680 after correction. The Ratio of minimum to maximum transmission is 0.8933. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       plate
_exptl_crystal_F_000             1062
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         2232
_refine_ls_number_restraints     1450
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.1333
_refine_ls_R_factor_gt           0.1314
_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^)+(0.0001P)^2^+100.0584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2770
_refine_ls_wR_factor_ref         0.2779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2188
_reflns_number_total             2232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           1_k_3thf_cr
_cod_depositor_comments
'Adding full bibliography for 7706910--7706927.cif.'
_cod_original_cell_volume        2898.0(8)
_cod_database_code               7706918
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.902
_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. Restrained distances
 C55-C56
 1.45 with sigma of 0.02
 C59-C60
 1.45 with sigma of 0.02
 K1-O3 \\sim K1-O4
 with sigma of 0.02
 O3-C61 \\sim O4-C65
 with sigma of 0.02
 O3-C58 \\sim O4-C62
 with sigma of 0.02
 C61-C60 \\sim C65-C64
 with sigma of 0.02
 C60-C59 \\sim C64-C63
 with sigma of 0.02
 C59-C58 \\sim C63-C62
 with sigma of 0.02
 K1-C61 \\sim K1-C65
 with sigma of 0.04
 K1-C58 \\sim K1-C62
 with sigma of 0.04
 O3-C60 \\sim O4-C64
 with sigma of 0.04
 O3-C59 \\sim O4-C63
 with sigma of 0.04
 C61-C59 \\sim C65-C63
 with sigma of 0.04
 C61-C58 \\sim C65-C62
 with sigma of 0.04
 C60-C58 \\sim C64-C62
 with sigma of 0.04
 Si2-C40 \\sim Si2-C43
 with sigma of 0.02
 C41-C40 \\sim C45-C43
 with sigma of 0.02
 C40-C42 \\sim C43-C44
 with sigma of 0.02
 Si2-C41 \\sim Si2-C45
 with sigma of 0.04
 Si2-C42 \\sim Si2-C44
 with sigma of 0.04
 C41-C42 \\sim C45-C44
 with sigma of 0.04
 Si1-C46 \\sim Si1-C47
 with sigma of 0.02
 C20-C46 \\sim C48-C47
 with sigma of 0.02
 C46-C21 \\sim C47-C49
 with sigma of 0.02
 Si1-C20 \\sim Si1-C48
 with sigma of 0.04
 Si1-C21 \\sim Si1-C49
 with sigma of 0.04
 C20-C21 \\sim C48-C49
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Cr1 \\sim Si1 \\sim Si2 \\sim N1 \\sim N2 \\sim C1 \\sim C2 \\sim C3 \\sim H3
\\sim C4 \\sim H4 \\sim C5 \\sim H5 \\sim C6 \\sim C7 \\sim H7 \\sim C8 \\sim
H8A \\sim H8B \\sim H8C \\sim C9 \\sim H9A \\sim H9B \\sim H9C \\sim C10 \\sim
H10 \\sim C11 \\sim H11A \\sim H11B \\sim H11C \\sim C12 \\sim H12B \\sim H12C
\\sim C13 \\sim H13 \\sim C14 \\sim H14A \\sim H14B \\sim H14C \\sim C15 \\sim
H15A \\sim H15B \\sim H15C \\sim C16 \\sim C17 \\sim H17A \\sim H17B \\sim C18
\\sim H18B \\sim H18C \\sim C22 \\sim C23 \\sim C24 \\sim H24 \\sim C25 \\sim
H25 \\sim C26 \\sim H26 \\sim C27 \\sim C28 \\sim H28 \\sim C29 \\sim H29A
\\sim H29B \\sim H29C \\sim C30 \\sim H30A \\sim H30B \\sim H30C \\sim C31
\\sim H31 \\sim C32 \\sim H32A \\sim H32B \\sim H32C \\sim C33 \\sim H33A \\sim
H33B \\sim H33C \\sim C34 \\sim H34 \\sim C35 \\sim H35A \\sim H35B \\sim H35C
\\sim C36 \\sim H36A \\sim H36B \\sim H36C \\sim C37 \\sim H37 \\sim C38 \\sim
H38A \\sim H38B \\sim H38C \\sim C39 \\sim H39B \\sim C20 \\sim C21 \\sim C40
\\sim C41 \\sim C42 \\sim C46: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C54) \\sim Ueq, Uanis(C55) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C57)
\\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(Cr1) \\sim Ueq, Uanis(Si2) \\sim Ueq, Uanis(Si1) \\sim Ueq, Uanis(N1)
\\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq,
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C37) \\sim Ueq,
Uanis(C20) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C40)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C39) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C46) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C36) \\sim Ueq, : with sigma of 0.1 and sigma for terminal
atoms of 0.2
Uanis(C22) = Uanis(C27) = Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C23)
Uanis(C1) = Uanis(C6) = Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2)
Uanis(C20) = Uanis(C46) = Uanis(C21)
Uanis(C61) = Uanis(C60) = Uanis(C59) = Uanis(C58) = Uanis(C50) = Uanis(C51) =
Uanis(C52) = Uanis(C53)
Uanis(O3) = Uanis(O1)
Uanis(O2) = Uanis(O4)
Uanis(C62) = Uanis(C63) = Uanis(C65) = Uanis(C64) = Uanis(C57) = Uanis(C56) =
Uanis(C55) = Uanis(C54)
Uanis(C45) = Uanis(C43) = Uanis(C44) = Uanis(C40) = Uanis(C41) = Uanis(C42)
Uanis(C21) = Uanis(C49) = Uanis(C46) = Uanis(C47) = Uanis(C20) = Uanis(C48) =
Uanis(C15) = Uanis(C13) = Uanis(C14)
4. Rigid body (RIGU) restrains
 O1, C50, C51, C52, C53
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C54, C55, C56, C57
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cr1, Si1, Si2, N1, N2, C1, C2, C3, H3, C4, H4, C5, H5, C6, C7, H7, C8, H8A,
 H8B, H8C, C9, H9A, H9B, H9C, C10, H10, C11, H11A, H11B, H11C, C12, H12B, H12C,
 C13, H13, C14, H14A, H14B, H14C, C15, H15A, H15B, H15C, C16, C17, H17A, H17B,
 C18, H18B, H18C, C22, C23, C24, H24, C25, H25, C26, H26, C27, C28, H28, C29,
 H29A, H29B, H29C, C30, H30A, H30B, H30C, C31, H31, C32, H32A, H32B, H32C, C33,
 H33A, H33B, H33C, C34, H34, C35, H35A, H35B, H35C, C36, H36A, H36B, H36C, C37,
 H37, C38, H38A, H38B, H38C, C39, H39B, C20, C21, C40, C41, C42, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O4)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=
 Sof(H64A)=Sof(H64B)=Sof(C65)=Sof(H65A)=Sof(H65B)=1-FVAR(1)
 Sof(O3)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C60)=
 Sof(H60A)=Sof(H60B)=Sof(C61)=Sof(H61A)=Sof(H61B)=FVAR(1)
 Fixed Sof: C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C21(0.5) H21A(0.5)
 H21B(0.5) H21C(0.5) C40(0.5) H40(0.5) C41(0.5) H41A(0.5) H41B(0.5) H41C(0.5)
 C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C46(0.5) H46(0.5) C43(0.5) H43(0.5)
 C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5)
 C47(0.5) H47(0.5) C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C49(0.5) H49A(0.5)
 H49B(0.5) H49C(0.5)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C28(H28), C31(H31), C34(H34), C37(H37), C40(H40),
 C46(H46), C43(H43), C47(H47)
6.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
 C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
  C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C24(H24), C25(H25), C26(H26)
6.d Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C1,C2), C22(C23,C24,C25,C26,C27)
6.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C)
;
_shelx_res_checksum              77594
_shelx_hkl_checksum              21967
_olex2_submission_special_instructions 'No special instructions were received'