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_7706919
_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 H34 Na O7'
_chemical_formula_sum            'C46 H86 Fe N2 Na O7 Si2'
_chemical_formula_weight         914.18
_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             2020-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-22 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                71.086(15)
_cell_angle_beta                 76.889(16)
_cell_angle_gamma                70.636(15)
_cell_formula_units_Z            2
_cell_length_a                   12.392(3)
_cell_length_b                   13.002(3)
_cell_length_c                   18.053(3)
_cell_measurement_reflns_used    10961
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.944
_cell_measurement_theta_min      1.725
_cell_volume                     2572.7(10)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'imaging plate area detector'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5 mm fibre optic'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2177
_diffrn_reflns_av_unetI/netI     0.1943
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            23621
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.944
_diffrn_reflns_theta_min         1.725
_diffrn_source                   'sealed X-ray tube, 12 x 0.4 mm LF focus'
_diffrn_source_target            Mo
_diffrn_source_type              'STOE C-Tech Mo LFF X-Ray Tube'
_exptl_absorpt_coefficient_mu    0.395
_exptl_absorpt_correction_T_max  0.7492
_exptl_absorpt_correction_T_min  0.1059
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Area X-Red32 1.63.4.0 (STOE, 2017)'
_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    1.180
_exptl_crystal_description       plate
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.893
_exptl_crystal_size_mid          0.503
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         10961
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.1415
_refine_ls_R_factor_gt           0.0828
_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^)+(0.1165P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.2306
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5693
_reflns_number_total             10961
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           7_na_18c6_fe
_cod_depositor_comments
'Adding full bibliography for 7706910--7706927.cif.'
_cod_database_code               7706919
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.720
_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. Uiso/Uaniso restraints and constraints
Uanis(O00B) \\sim Ueq, Uanis(O00C) \\sim Ueq, Uanis(O007) \\sim Ueq,
Uanis(O008) \\sim Ueq, Uanis(O00D) \\sim Ueq, Uanis(O006) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O00B) \\sim Ueq, Uanis(C01K) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C0AA) \\sim Ueq, Uanis(C11) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C01K) = Uanis(C01H)
Uanis(O006) = Uanis(O007) = Uanis(O005) = Uanis(O00C) = Uanis(O00B) =
Uanis(O00D) = Uanis(O008)
3. Others
 Fixed Sof: O00B(0.5) O00C(0.5) O00D(0.5) HM(0.5) HN(0.5) H5AA(0.5) HO(0.5)
 H6AA(0.5) HP(0.5) HQ(0.5) HR(0.5) C01K(0.5) H7AA(0.5) HS(0.5) C01N(0.5)
 H8AA(0.5) HT(0.5) C11(0.5) H11A(0.5) H11B(0.5) C0AA(0.5) H0AB(0.5) H0AC(0.5)
 C1A(0.5) H1AB(0.5) H1AC(0.5) C18(0.5) H18A(0.5) H18B(0.5) O8(0.5) O9(0.5)
 C1AA(0.5) H1AD(0.5) H1AE(0.5) C2AA(0.5) H2AB(0.5) H2AC(0.5) C3AA(0.5)
 H3AB(0.5) H3AC(0.5) C3(0.5) H3A(0.5) H3B(0.5) O1(0.5)
4.a Ternary CH refined with riding coordinates:
 C00I(H00I), C00N(H00N), C00O(H00O), C010(H010)
4.b Secondary CH2 refined with riding coordinates:
 C00T(H00Y,H), C00Y(H00Z,HA), C016(H01,HD), C017(H0AA,HE), C019(H1AA,HF),
 C01C(H2AA,HG), C01E(H3AA,HH), C01H(HM,HN), C01H(H5AA,HO), C01I(H6AA,HP),
 C01I(HQ,HR), C01K(H7AA,HS), C01N(H8AA,HT), C11(H11A,H11B), C0AA(H0AB,H0AC),
 C1A(H1AB,H1AC), C18(H18A,H18B), C1AA(H1AD,H1AE), C2AA(H2AB,H2AC), C3AA(H3AB,
 H3AC), C3(H3A,H3B)
4.c Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00K(H00K), C00L(H00L), C00U(H00U), C00V(H00V), C00X(H00X)
4.d Idealised Me refined as rotating group:
 C00P(H00A,H00B,H00C), C00Q(H00D,H00E,H00F), C00S(H00G,H00J,H00M), C00W(H00P,
 H00Q,H00R), C00Z(H00S,H00T,H00W), C011(H01A,H01B,H01C), C012(H01D,H01E,H01F),
 C013(H01Z,HB,HC), C014(H01G,H01H,H01I), C015(H01J,H01K,H01L), C018(H01M,H01N,
 H01O), C01A(H01P,H01Q,H01R), C01B(H01S,H01T,H01U), C01D(H01V,H01W,H01X),
 C01F(H01Y,HI,HJ), C01G(H4AA,HK,HL)
;
_shelx_res_checksum              91353
_shelx_hkl_checksum              35533
_olex2_submission_special_instructions 'No special instructions were received'