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_7706913
_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 Co N2 Si2, C16 H36 N'
_chemical_formula_sum            'C46 H88 Co N3 Si2'
_chemical_formula_weight         798.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-06-17
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7553(6)
_cell_length_b                   19.9389(8)
_cell_length_c                   22.5989(11)
_cell_measurement_reflns_used    21067
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.995
_cell_measurement_theta_min      1.34
_cell_volume                     4846.3(4)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36221
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.802
_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    0.435
_exptl_absorpt_correction_T_max  0.9593
_exptl_absorpt_correction_T_min  0.4100
_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. = 0.587 (run 2)   max. = 1.373 (run 1)    spread = 0.8
;
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_description       block
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.185
_exptl_crystal_size_rad          0.062
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.152(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         8508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0422P)^2^+1.1788P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                8046
_reflns_number_total             8508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00121c2.cif
_cod_data_source_block           9_bu4nco
_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 Co4 N12 Si8'
_cod_original_formula_weight         3193.20
_cod_original_formula_moiety         '4(C30 H52 Co N2 Si2), 4(C16 H36 N)'
_cod_original_formula_units_Z            1
_cod_database_code               7706913
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.834
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.848(12)
 0.152(12)
2. 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
3.a Ternary CH refined with riding coordinates:
 C00A(H00A), C00F(H00F), C00R(H00R), C018(H018)
3.b Secondary CH2 refined with riding coordinates:
 C00D(H00,H), C00H(H0AA,HA), C00K(H1AA,HB), C00L(H2AA,HC), C00M(H3AA,HD),
 C00U(H4AA,HE), C00W(H5AA,HF), C00Z(H6AA,HI), C011(H01W,H01X), C012(H01Y,HJ),
 C017(H01,HM), C01E(H9AA,HR)
3.c Aromatic/amide H refined with riding coordinates:
 C009(H009), C00C(H00C), C00E(H00E), C00I(H00I), C00V(H00V), C01B(H01M)
3.d Idealised Me refined as rotating group:
 C00J(H00B,H00D,H00G), C00N(H00H,H00J,H00K), C00Q(H00L,H00M,H00N), C00S(H00O,
 H00P,H00Q), C00T(H00S,H00T,H00U), C00X(H00W,H00X,H00Y), C00Y(H00Z,HG,HH),
 C010(H01A,H01B,H01C), C013(H01D,H01E,H01F), C014(H01G,H01H,H01I), C015(H01Z,HK,
 HL), C016(H01J,H01K,H01L), C019(H7AA,HN,HO), C01A(H8AA,HP,HQ), C01C(H01N,H01O,
 H01P), C01D(H01Q,H01R,H01S), C01F(H0BA,HS,HT), C01G(H01T,H01U,H01V)
;
_shelx_res_checksum              52354
_shelx_hkl_checksum              30948
_olex2_submission_special_instructions 'No special instructions were received'