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_1556440
_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 Fe N4 Si4, 2(C10 H20 K0.5 O4)'
_chemical_formula_sum            'C42 H84 Fe K N4 O8 Si4'
_chemical_formula_weight         980.44
_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                77.5970(10)
_cell_angle_beta                 80.062(2)
_cell_angle_gamma                83.452(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8613(5)
_cell_length_b                   13.2627(6)
_cell_length_c                   19.8669(9)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.4988
_cell_measurement_theta_min      2.3440
_cell_volume                     2744.3(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_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 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Quest D8'
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            103782
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.562
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'ADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1663 before and 0.0332 after correction. The Ratio of minimum to maximum transmission is 0.950. The \l/2 correction factor is Not present.'
_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    1.187
_exptl_crystal_description       prism
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         12642
_refine_ls_number_restraints     560
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0266P)^2^+1.2231P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10773
_reflns_number_total             12642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            K_18c6_Fe3.cif
_cod_data_source_block           k(18c6)fe7
_cod_database_code               1556440
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.905
_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. Uiso/Uaniso restraints and constraints
O1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim O1SA \\sim C2SA \\sim C3SA
\\sim C4SA \\sim C5SA: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
O1S' \\sim C2S' \\sim C3S' \\sim C4S' \\sim C5S' \\sim O1SB \\sim C2SB \\sim
C3SB \\sim C4SB \\sim C5SB: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(O1S) \\sim Ueq, Uanis(C2S) \\sim Ueq, Uanis(C3S) \\sim Ueq, Uanis(C4S)
\\sim Ueq, Uanis(C5S) \\sim Ueq, Uanis(O1SA) \\sim Ueq, Uanis(C2SA) \\sim Ueq,
Uanis(C3SA) \\sim Ueq, Uanis(C4SA) \\sim Ueq, Uanis(C5SA) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(O1S') \\sim Ueq, Uanis(C2S') \\sim Ueq, Uanis(C3S') \\sim Ueq,
Uanis(C4S') \\sim Ueq, Uanis(C5S') \\sim Ueq, Uanis(O1SB) \\sim Ueq,
Uanis(C2SB) \\sim Ueq, Uanis(C3SB) \\sim Ueq, Uanis(C4SB) \\sim Ueq,
Uanis(C5SB) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 O1S, C2S, C3S, C4S, C5S, O1SA, C2SA, C3SA, C4SA, C5SA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1S', C2S', C3S', C4S', C5S', O1SB, C2SB, C3SB, C4SB, C5SB
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{O1SA, C2SA, C3SA, C4SA, C5SA} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1S, C2S, C3S, C4S, C5S}
{O1SB, C2SB, C3SB, C4SB, C5SB} sigma for 1-2: 0.02, 1-3: 0.04
as
{O1S', C2S', C3S', C4S', C5S'}
5. Others
 Sof(O1SA)=Sof(C2SA)=Sof(H2SG)=Sof(H2SH)=Sof(C3SA)=Sof(H3SG)=Sof(H3SH)=
 Sof(C4SA)=Sof(H4SG)=Sof(H4SH)=Sof(C5SA)=Sof(H5SG)=Sof(H5SH)=1-FVAR(1)
 Sof(O1S)=Sof(C2S)=Sof(H2SE)=Sof(H2SF)=Sof(C3S)=Sof(H3SE)=Sof(H3SF)=Sof(C4S)=
 Sof(H4SE)=Sof(H4SF)=Sof(C5S)=Sof(H5SE)=Sof(H5SF)=FVAR(1)
 Sof(O1SB)=Sof(C2SB)=Sof(H2SC)=Sof(H2SD)=Sof(C3SB)=Sof(H3SC)=Sof(H3SD)=
 Sof(C4SB)=Sof(H4SC)=Sof(H4SD)=Sof(C5SB)=Sof(H5SC)=Sof(H5SD)=1-FVAR(2)
 Sof(O1S')=Sof(C2S')=Sof(H2SA)=Sof(H2SB)=Sof(C3S')=Sof(H3SA)=Sof(H3SB)=
 Sof(C4S')=Sof(H4SA)=Sof(H4SB)=Sof(C5S')=Sof(H5SA)=Sof(H5SB)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C2C(H2CA,H2CB), C3C(H3CA,H3CB), C5C(H5CA,H5CB), C6C(H6CA,H6CB), C8C(H8CA,
 H8CB), C9C(H9CA,H9CB), C2K(H2KA,H2KB), C3K(H3KA,H3KB), C5K(H5KA,H5KB),
 C6K(H6KA,H6KB), C8K(H8KA,H8KB), C9K(H9KA,H9KB), C2S(H2SE,H2SF), C3S(H3SE,H3SF),
  C4S(H4SE,H4SF), C5S(H5SE,H5SF), C2SA(H2SG,H2SH), C3SA(H3SG,H3SH), C4SA(H4SG,
 H4SH), C5SA(H5SG,H5SH), C2S'(H2SA,H2SB), C3S'(H3SA,H3SB), C4S'(H4SA,H4SB),
 C5S'(H5SA,H5SB), C2SB(H2SC,H2SD), C3SB(H3SC,H3SD), C4SB(H4SC,H4SD), C5SB(H5SC,
 H5SD)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
6.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C)
;
_shelx_res_checksum              51555
_shelx_hkl_checksum              12399
_olex2_submission_special_instructions 'No special instructions were received'