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_7706914
_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 K N2 Si2'
_chemical_formula_sum            'C30 H52 Fe K N2 Si2'
_chemical_formula_weight         591.86
_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
_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                115.309(2)
_cell_angle_beta                 91.001(2)
_cell_angle_gamma                110.473(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8776(6)
_cell_length_b                   14.0736(7)
_cell_length_c                   14.4037(7)
_cell_measurement_reflns_used    9122
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.999
_cell_measurement_theta_min      2.204
_cell_volume                     1999.11(18)
_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 0.998
_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  0.0405
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            72350
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.867
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1559 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.9209.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.983
_exptl_crystal_description       block
_exptl_crystal_F_000             638
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.386
_exptl_crystal_size_min          0.278
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0471P)^2^+0.8431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7064
_reflns_number_total             7861
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           3_kfe
_cod_depositor_comments
'Adding full bibliography for 7706910--7706927.cif.'
_cod_database_code               7706914
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.768
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H) groups, All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H)
2.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00J(H00J), C00K(H00K)
2.c Idealised Me refined as rotating group:
 C00O(H00A,H00B,H00C), C00P(H00D,H00O,H00P), C00Q(H00Q,H00R,H00S), C00R(H00T,
 H00U,H00V), C00S(H00W,H00X,H00Y), C00T(H00Z,H,HA), C00U(H00,HB,HC), C00V(H0AA,
 HD,HE), C00W(H1AA,HF,HG), C00X(H2AA,HH,HI), C00Y(H3AA,HJ,HK), C00Z(H4AA,HL,HM),
  C010(H01A,H01B,H01C)
;
_shelx_res_checksum              74753
_shelx_hkl_checksum              99856
_shelx_fab_checksum              29538
_olex2_submission_special_instructions 'No special instructions were received'