Reduction of 2,2'-Bipyridine by Quasi-Linear 3d-Metal(I) Silylamides-A Structural and Spectroscopic Study
Muller, I.; Schneider, C.; Pietzonka, C.; Kraus, F.; Werncke, C.G.; Inorganics 7 (2019) 117–; doi:10.3390/inorganics7100117

data_1556438
_publ_section_title
;
 Reduction of 2,2'-Bipyridine by Quasi-Linear 3d-Metal(I) Silylamides-A
 Structural and Spectroscopic Study
;
_journal_name_full               Inorganics
_journal_page_first              117
_journal_paper_doi               10.3390/inorganics7100117
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C22 H44 Co N4 Si4, 2(C10 H20 K0.5 O4)'
_chemical_formula_sum            'C42 H84 Co K N4 O8 Si4'
_chemical_formula_weight         983.52
_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
_cell_angle_alpha                77.712(2)
_cell_angle_beta                 80.199(2)
_cell_angle_gamma                83.606(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8097(5)
_cell_length_b                   13.2648(6)
_cell_length_c                   19.9051(10)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.7563
_cell_measurement_theta_min      2.3772
_cell_volume                     2739.7(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_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  0.0853
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            89930
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.529
_diffrn_reflns_theta_min         2.119
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       plate
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         12549
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0280P)^2^+1.5905P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9015
_reflns_number_total             12549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            K_18c6_Co4.cif
_cod_data_source_block           k(18c6)co8
_cod_database_code               1556438
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.889
_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. Rigid body (RIGU) restrains
 O100, C101, C102, C103, C104, O200, C201, C204
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H10E)=Sof(H10F)=Sof(H10I)=Sof(H10J)=Sof(O200)=Sof(C201)=Sof(H20A)=
 Sof(H20B)=Sof(C204)=Sof(H20C)=Sof(H20D)=1-FVAR(1)
 Sof(O100)=Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(H10D)=Sof(H10G)=
 Sof(H10H)=Sof(C104)=Sof(H10K)=Sof(H10L)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C2C(H2CA,H2CB), C3C(H3CA,H3CB), C5C(H5CA,H5CB), C6C(H6CA,H6CB), C8C(H8CA,
 H8CB), C16C(H16C,H16D), C2K(H2KA,H2KB), C3K(H3KA,H3KB), C5K(H5KA,H5KB),
 C6K(H6KA,H6KB), C8K(H8KA,H8KB), C16K(H16A,H16B), C301(H30A,H30B), C302(H30C,
 H30D), C303(H30E,H30F), C304(H30G,H30H), C101(H10A,H10B), C102(H10C,H10D),
 C102(H10E,H10F), C103(H10G,H10H), C103(H10I,H10J), C104(H10K,H10L), C201(H20A,
 H20B), C204(H20C,H20D)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
4.c Idealised Me refined as rotating group:
 C111(H11A,H11B,H11C), C112(H11D,H11E,H11F), C113(H11G,H11H,H11I), C121(H12A,
 H12B,H12C), C122(H12D,H12E,H12F), C123(H12G,H12H,H12I), C211(H21A,H21B,H21C),
 C212(H21D,H21E,H21F), C213(H21G,H21H,H21I), C221(H22A,H22B,H22C), C222(H22D,
 H22E,H22F), C223(H22G,H22H,H22I)
;
_shelx_res_checksum              4934
_shelx_hkl_checksum              90450
_olex2_submission_special_instructions 'No special instructions were received'