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_1556437
_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_absolute_configuration ad
_chemical_formula_moiety         'C22 H44 Co N4 Si4'
_chemical_formula_sum            'C22 H44 Co N4 Si4'
_chemical_formula_weight         535.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7674(9)
_cell_length_b                   18.1030(8)
_cell_length_c                   17.5930(7)
_cell_measurement_reflns_used    28582
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      1.485
_cell_volume                     5977.2(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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20518
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.945
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.9352
_exptl_absorpt_correction_T_min  0.8292
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-Area'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_description       block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.495(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         10939
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0307
_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^)+(0.0514P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.866
_reflns_Friedel_fraction_max     0.860
_reflns_number_gt                10341
_reflns_number_total             10939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Co8.cif
_cod_data_source_block           co4
_cod_database_code               1556437
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.801
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.505(10)
 0.495(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C7A(H7A), C8A(H8A), C9A(H9A),
 C10A(H10A), C1B(H1B), C2B(H2B), C3B(H3B), C7B(H7B), C8B(H8B), C9B(H9B),
 C10B(H10B)
3.b Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C12A(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C14A(H14A,
 H14B,H14C), C15A(H15A,H15B,H15C), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C),
 C18A(H18A,H18B,H18C), C19A(H19A,H19B,H19C), C20A(H20A,H20B,H20C), C21A(H21A,
 H21B,H21C), C22A(H22A,H22B,H22C), C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F),
 C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F), C15B(H15D,H15E,H15F), C16B(H16D,
 H16E,H16F), C17B(H17D,H17E,H17F), C18B(H18D,H18E,H18F), C19B(H19D,H19E,H19F),
 C20B(H20D,H20E,H20F), C21B(H21D,H21E,H21F), C22B(H22D,H22E,H22F)
;
_shelx_res_checksum              52427
_shelx_hkl_checksum              60908
_olex2_submission_special_instructions 'No special instructions were received'