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_7706916
_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 H36 N'
_chemical_formula_sum            'C46 H88 Fe N3 Si2'
_chemical_formula_weight         795.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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
;
2020-06-18 deposited with the CCDC.	2021-03-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.323(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.298(2)
_cell_length_b                   13.8270(10)
_cell_length_c                   21.446(3)
_cell_measurement_reflns_used    10436
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.739
_cell_measurement_theta_min      2.431
_cell_volume                     4944.4(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    'ShelXT (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 0.992
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_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  0.0656
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            41152
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.739
_diffrn_reflns_theta_min         2.431
_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    0.385
_exptl_absorpt_correction_T_max  0.9713
_exptl_absorpt_correction_T_min  0.8944
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
X-Area X-Red32 1.63.4.0 (STOE, 2017)      Statistics over combined scale factors for x file reflections:
       min. = 0.847 (run 1)   max. = 1.106 (run 2)    spread = 0.3
;
_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    1.068
_exptl_crystal_description       plate
_exptl_crystal_F_000             1756
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.173
_exptl_crystal_size_rad          0.062
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         10436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.1757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6920
_reflns_number_total             10436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           8_bu4nfe
_cod_depositor_comments
;
Adding full bibliography for 7706910--7706927.cif.

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C184 H352 Fe4 N12 Si8'
_cod_original_formula_weight         3180.87
_cod_original_formula_moiety         '4(C30 H52 Fe N2 Si2), 4(C16 H36 N)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        4944.3(10)
_cod_database_code               7706916
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.870
_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.a Ternary CH refined with riding coordinates:
 C00I(H00I), C00J(H00J), C010(H010), C013(H013)
2.b Secondary CH2 refined with riding coordinates:
 C00C(H00Q,H00R), C00F(H00S,H00U), C00G(H00V,H00W), C00K(H00Y,H), C00L(H00Z,
 HA), C00M(H00,HB), C00N(H0AA,HC), C00S(H2AA,HF), C00W(H5AA,HK), C00Y(H6AA,HL),
 C016(H01,HM), C018(H7AA,HN)
2.c Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00H(H00H), C00T(H00T), C00X(H00X), C012(H012), C015(H015)
2.d Idealised Me refined as rotating group:
 C00O(H00A,H00B,H00C), C00P(H00E,H00F,H00G), C00Q(H00K,H00L,H00M), C00R(H1AA,
 HD,HE), C00U(H3AA,HG,HH), C00V(H4AA,HI,HJ), C00Z(H00N,H00O,H00P), C011(H01A,
 H01B,H01C), C014(H01D,H01E,H01F), C017(H01G,H01H,H01I), C019(H01J,H01K,H01L),
 C01A(H01M,H01N,H01O), C01B(H01P,H01Q,H01R), C01C(H01S,H01T,H01U), C01D(H01V,
 H01W,H01X), C01E(H01Y,HO,HP), C01F(H01Z,HQ,HR), C01G(H8AA,HS,HT)
;
_shelx_res_checksum              94266
_shelx_hkl_checksum              14137
_olex2_submission_special_instructions 'No special instructions were received'