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_7709852
_publ_section_title
;
 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         '2(C36 H28 Co Ni O2 P2), Cl6 Fe2 O'
_chemical_formula_sum            'C72 H56 Cl6 Co2 Fe2 Ni2 O5 P4'
_chemical_formula_weight         1684.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2019-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-26 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                68.911(3)
_cell_angle_beta                 80.097(4)
_cell_angle_gamma                74.415(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1357(5)
_cell_length_b                   17.5973(8)
_cell_length_c                   21.6427(11)
_cell_measurement_reflns_used    46677
_cell_measurement_temperature    135
_cell_measurement_theta_max      66.65
_cell_measurement_theta_min      2.20
_cell_volume                     3457.0(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      135.0
_diffrn_measured_fraction_theta_full 0.9613
_diffrn_measured_fraction_theta_max 0.9613
_diffrn_measurement_device_type  'Apex II, Brucker'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1107
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46677
_diffrn_reflns_theta_full        66.6518
_diffrn_reflns_theta_max         66.65
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    10.952
_exptl_absorpt_correction_T_max  0.8642
_exptl_absorpt_correction_T_min  0.6452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'R.H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.6184
_exptl_crystal_description       block
_exptl_crystal_F_000             1688.2647
_exptl_crystal_preparation       'see manuscript'
_exptl_crystal_recrystallization_method 'slow evaporation of DCM'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.8483
_refine_diff_density_min         -0.9417
_refine_diff_density_rms         0.2064
_refine_ls_d_res_high            0.8396
_refine_ls_d_res_low             20.1221
_refine_ls_goodness_of_fit_ref   1.0220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    112
_refine_ls_number_parameters     838
_refine_ls_number_reflns         11746
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0220
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.5841P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              20
_reflns_limit_k_min              -18
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                7525
_reflns_number_total             11746
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2dt00650b11.cif
_cod_data_source_block           ac465a
_cod_depositor_comments
;

2025-03-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C36 H28 Cl3 Co Fe Ni O2.5 P2'
_cod_original_formula_weight         842.40
_cod_original_formula_moiety         'C36 H28 Co Ni O2 P2, 0.5(Cl6 Fe2 O)'
_cod_original_formula_units_Z            4
_cod_database_code               7709852
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4a(H4a), C5a(H5a), C6a(H6a), C7a(H7a), C9a(H9a), C10a(H10a), C11a(H11a),
 C12a(H12a), C14a(H14a), C15a(H15a), C16a(H16a), C17a(H17a), C18a(H18a),
 C20a(H20a), C21a(H21a), C22a(H22a), C23a(H23a), C24a(H24a), C26a(H26a),
 C27a(H27a), C28a(H28a), C29a(H29a), C30a(H30a), C32a(H32a), C33a(H33a),
 C34a(H34a), C35a(H35a), C36a(H36a), C4b(H4b), C5b(H5b), C6b(H6b), C7b(H7b),
 C9b(H9b), C10b(H10b), C11b(H11b), C12b(H12b), C14b(H14b), C15b(H15b),
 C16b(H16b), C17b(H17b), C18b(H18b), C20b(H20b), C21b(H21b), C22b(H22b),
 C23b(H23b), C24b(H24b), C26b(H26b), C27b(H27b), C28b(H28b), C29b(H29b),
 C30b(H30b), C32b(H32b), C33b(H33b), C34b(H34b), C35b(H35b), C36b(H36b)
;
_olex2_submission_special_instructions 'No special instructions were received'