Metal-Metal Communication Between 1,1’ Bis(diphenylphosphino)cobaltocenium and an Organonickel Moiety
Auweiler, Daniel; Schnierle, Marc; Rapp, Valentin; Ringenberg, Mark R.; Dalton Transactions  (2022) –; doi:10.1039/D2DT00650B

data_7709854
_publ_section_title
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 Metal-Metal Communication Between 1,1&#x2019;
 Bis(diphenylphosphino)cobaltocenium and an Organonickel Moiety
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00650B
_journal_year                    2022
_chemical_formula_moiety         'C39 H33 Co Ni P2, 2(B F4)'
_chemical_formula_sum            'C39 H33 B2 Co F8 Ni P2'
_chemical_formula_weight         854.85
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-29 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.827(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0540(14)
_cell_length_b                   10.2096(8)
_cell_length_c                   20.0648(16)
_cell_measurement_reflns_used    56875
_cell_measurement_temperature    140
_cell_measurement_theta_max      25.242
_cell_measurement_theta_min      2.032
_cell_volume                     3489.3(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      139.99
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Apex II, Brucker'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            56875
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.518
_diffrn_reflns_theta_min         2.032
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  0.8035
_exptl_absorpt_correction_T_min  0.5837
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
J. de Meulenaar and H. Tompa, Acta Crystallogr., Sect A 1965, 19, 1014-1018.
P. Coppens in Crystallographic Computing ed F.R. Ahmed, S.R. Hall and C.P. Huber, Copenhagen, Munksgaard, (1970) pp 255-270
;
_exptl_crystal_colour            brown-yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_preparation       'see manuscript'
_exptl_crystal_recrystallization_method
'from slow evaporation of CH2Cl2 solution'
_exptl_crystal_size_max          0.536
_exptl_crystal_size_mid          0.514
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.776
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         10610
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+3.3520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8707
_reflns_number_total             10610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00650b11.cif
_cod_data_source_block           ac535
_cod_database_code               7709854
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.790
_shelx_estimated_absorpt_t_min   0.570
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C17B-C22A \\sim C17B-C22B
 with sigma of 0.02
 C17B-C18A \\sim C17B-C18B
 with sigma of 0.02
 C22A-C21A \\sim C22B-C21B
 with sigma of 0.02
 C21A-C20A \\sim C21B-C20B
 with sigma of 0.02
 C20A-C19A \\sim C20B-C19B
 with sigma of 0.02
 C18A-C19A \\sim C18B-C19B
 with sigma of 0.02
 C17B-C21A \\sim C17B-C21B
 with sigma of 0.04
 C17B-C19A \\sim C17B-C19B
 with sigma of 0.04
 C22A-C20A \\sim C22B-C20B
 with sigma of 0.04
 C21A-C19A \\sim C21B-C19B
 with sigma of 0.04
 C20A-C18A \\sim C20B-C18B
 with sigma of 0.04
 F11-B2 \\sim F10-B2
 with sigma of 0.02
 F8-B2 \\sim F9-B2
 with sigma of 0.02
 F7-B2 \\sim F6-B2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F11) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C17B) \\sim Ueq, Uanis(C18B) \\sim Ueq, Uanis(C19B) \\sim Ueq,
Uanis(C20B) \\sim Ueq, Uanis(C21B) \\sim Ueq, Uanis(C22B) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=
 Sof(H21B)=Sof(C22B)=Sof(H22B)=1-FVAR(1)
 Sof(C21A)=Sof(H21A)=Sof(C20A)=Sof(H20A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=
 Sof(H19A)=Sof(C22A)=Sof(H22A)=FVAR(1)
 Sof(F6)=Sof(F9)=Sof(F10)=1-FVAR(2)
 Sof(F8)=Sof(F7)=Sof(F11)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10),
 C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18B(H18B), C19B(H19B),
 C20B(H20B), C21B(H21B), C22B(H22B), C24(H24), C25(H25), C26(H26), C27(H27),
 C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37),
  C38(H38), C39(H39), C21A(H21A), C20A(H20A), C18A(H18A), C19A(H19A), C22A(H22A)
5.b Fitted hexagon refined as free rotating group:
 C17B(C18B,C19B,C20B,C21B,C22B)
;
_olex2_exptl_crystal_mounting_method
'mounted in perfluoropolyether cryo oil onto a cryoloop'
_olex2_submission_special_instructions 'No special instructions were received'