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_1556439
_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 Cr N4 Si4, C20 H40 K O8'
_chemical_formula_sum            'C42 H84 Cr K N4 O8 Si4'
_chemical_formula_weight         976.59
_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
_atom_sites_solution_primary     direct
_cell_angle_alpha                95.633(2)
_cell_angle_beta                 89.8920(10)
_cell_angle_gamma                90.377(2)
_cell_formula_units_Z            4
_cell_length_a                   11.6269(2)
_cell_length_b                   21.5546(4)
_cell_length_c                   21.8560(4)
_cell_measurement_reflns_used    124112
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      1.75
_cell_volume                     5450.83(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            106690
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.752
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.8481
_exptl_absorpt_correction_T_min  0.6245
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Area X-Red 1.63.1.0 (STOE, 2016)'
_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    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.3494
_exptl_crystal_size_mid          0.2903
_exptl_crystal_size_min          0.2027
_refine_diff_density_max         1.019
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1112
_refine_ls_number_reflns         23726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0409P)^2^+12.4696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1502
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                20467
_reflns_number_total             23726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            K_18c6_Cr1.cif
_cod_data_source_block           k(18c6)cr5
_cod_database_code               1556439
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.867
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6437(8)
 0.3563(8)
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 Secondary CH2 refined with riding coordinates:
 C01G(H01A,H01B), C01K(H01C,H01D), C01Q(H01E,H01F), C02G(H02A,H02B), C02K(H02C,
 H02D), C02N(H02E,H02F), C02W(H02G,H02H), C024(H02I,H02J), C028(H02K,H02L),
 C033(H03A,H03B), C01A(H01G,H01H), C01B(H01I,H01J), C01D(H01K,H01L), C01H(H01M,
 H01N), C01R(H01O,H01P), C02L(H02M,H02N), C015(H01Q,H01R), C018(H01S,H01T),
 C027(H02O,H02P), C029(H02Q,H02R), C01O(H01U,H01V), C01Y(H01W,H01X), C02A(H02S,
 H02T), C02P(H02U,H02V), C02T(H02W,H02X), C02V(H02Y,H), C03B(H03C,H03D),
 C03D(H03E,H03F), C023(H02Z,HA), C030(H03G,H03H), C01E(H01Y,HB), C01F(H01Z,HC),
 C01I(H01,HD), C01M(H0AA,HE), C02C(H02,HF), C02F(H1AA,HG), C02Z(H2AA,HH),
 C03A(H03I,H03J), C03C(H03K,H03L), C020(H3AA,HI)
3.b 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), C4B(H4B), C7B(H7B), C8B(H8B),
 C9B(H9B), C10B(H10B)
3.c 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              7331
_shelx_hkl_checksum              73221
_olex2_submission_special_instructions 'No special instructions were received'