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_7706917
_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         'C42 H76 Fe K N2 O6 Si2, C4 H10 O'
_chemical_formula_sum            'C46 H88 Fe K N2 O7 Si2'
_chemical_formula_weight         930.29
_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                 95.062(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3333(7)
_cell_length_b                   34.0397(14)
_cell_length_c                   15.5254(9)
_cell_measurement_reflns_used    11480
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.811
_cell_measurement_theta_min      2.472
_cell_volume                     5439.6(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 0.984
_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  0.0441
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42532
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.811
_diffrn_reflns_theta_min         2.472
_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    0.442
_exptl_absorpt_correction_T_max  0.9593
_exptl_absorpt_correction_T_min  0.4995
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
X-Area LANA 1.71.6.0 (STOE, 2017)    Statistics over combined scale factors for x file reflections:
       min. = 0.692 (run 2)   max. = 1.330 (run 1)    spread = 0.6
;
_exptl_crystal_colour            'clear orangish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_description       needle
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.888
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.225
_exptl_crystal_size_rad          0.062
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         11480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0630P)^2^+1.2408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8430
_reflns_number_total             11480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           k_18c6_fe_et2o
_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 H344 Fe4 K4 N8 O28 Si8'
_cod_original_formula_weight         3721.17
_cod_original_formula_moiety         '4(C42 H76 Fe K N2 O6 Si2), 4(C4 H10 O)'
_cod_original_formula_units_Z            1
_cod_database_code               7706917
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.695
_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:
 C00U(H00U), C00V(H00V), C00Y(H00Y), C012(H012)
2.b Secondary CH2 refined with riding coordinates:
 C00L(H00D,H00E), C00N(H00F,H00G), C00O(H00H,H00I), C00S(H00O,H00P), C00X(H00Q,
 H00S), C00Z(H00X,H00Z), C013(H6AA,H), C014(H7AA,HA), C016(H01G,H01H),
 C019(H01O,H01P), C01A(H01Q,H01R), C01G(H0AA,HH), C01M(H4AA,HS), C01N(H5AA,HT)
2.c Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00M(H00M), C00R(H00R), C00T(H00T), C00W(H00W), C010(H010)
2.d Idealised Me refined as rotating group:
 C00G(H00A,H00B,H00C), C00Q(H00K,H00L,H00N), C011(H01A,H01B,H01C), C015(H01D,
 H01E,H01F), C017(H01I,H01J,H01K), C018(H01L,H01M,H01N), C01B(H01S,H01T,H01U),
 C01C(H01V,H01W,H01X), C01D(H01Y,HB,HC), C01E(H01Z,HD,HE), C01F(H01,HF,HG),
 C01H(H8AA,HI,HJ), C01I(H1AA,HK,HL), C01J(H2AA,HM,HN), C01K(H3AA,HO,HP),
 C01L(H9AA,HQ,HR)
;
_shelx_res_checksum              54820
_shelx_hkl_checksum              52272
_olex2_submission_special_instructions 'No special instructions were received'