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_7709855
_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         'C36 H28 Co Ni O2 P2, F6 P, C H2 Cl2'
_chemical_formula_sum            'C37 H30 Cl2 Co F6 Ni O2 P3'
_chemical_formula_weight         902.06
_chemical_properties_physical    Hygroscopic
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-30 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.232(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8614(11)
_cell_length_b                   12.6538(9)
_cell_length_c                   40.759(3)
_cell_measurement_reflns_used    71525
_cell_measurement_temperature    140
_cell_measurement_theta_max      28.373
_cell_measurement_theta_min      2.002
_cell_volume                     8167.6(10)
_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      140.01
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Apex II, Brucker'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            71525
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.373
_diffrn_reflns_theta_min         2.002
_exptl_absorpt_coefficient_mu    1.174
_exptl_absorpt_correction_T_max  0.9280
_exptl_absorpt_correction_T_min  0.6377
_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 red'
_exptl_crystal_colour_modifier   brown
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             3648
_exptl_crystal_preparation       'see manuscript'
_exptl_crystal_recrystallization_method 'obtained from CH2Cl2 evaporation'
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.353
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         10165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0234P)^2^+44.8323P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1095
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8592
_reflns_number_total             10165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00650b11.cif
_cod_data_source_block           ac539_sqd
_cod_database_code               7709855
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.585
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
;
_olex2_exptl_crystal_mounting_method
'mounted on to a cryoloop with perfluoropolyether cryo oil'
_olex2_submission_special_instructions 'No special instructions were received'