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_7709853
_publ_section_title
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 Metal-Metal Communication Between 1,1&#x2019;
 Bis(diphenylphosphino)cobaltocenium and an Organonickel Moiety
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00650B
_journal_year                    2022
_chemical_formula_moiety         'C39 H33 Co Ni P2, 1.58(F6 P), 0.42(B F4)'
_chemical_formula_sum            'C39 H33 B0.42 Co F11.16 Ni P3.58'
_chemical_formula_weight         946.84
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-03-22 deposited with the CCDC.	2022-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.858(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.107(2)
_cell_length_b                   10.7707(12)
_cell_length_c                   18.508(2)
_cell_measurement_reflns_used    52737
_cell_measurement_temperature    139.99
_cell_measurement_theta_max      26.43
_cell_measurement_theta_min      2.15
_cell_volume                     3781.6(7)
_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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      139.99
_diffrn_measured_fraction_theta_full 0.9880
_diffrn_measured_fraction_theta_max 0.9819
_diffrn_measurement_device_type  'Apex II, Brucker'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1029
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.9880
_diffrn_reflns_Laue_measured_fraction_max 0.9819
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            52737
_diffrn_reflns_point_group_measured_fraction_full 0.9880
_diffrn_reflns_point_group_measured_fraction_max 0.9819
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  0.8885
_exptl_absorpt_correction_T_min  0.6526
_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            'light green'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       needle
_exptl_crystal_F_000             1965.813
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/n-hexanes'
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.077
_refine_diff_density_max         3.093
_refine_diff_density_min         -2.580
_refine_diff_density_rms         0.248
_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     410
_refine_ls_number_reflns         7711
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1822
_refine_ls_R_factor_gt           0.1324
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1687P)^2^+84.3708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3256
_refine_ls_wR_factor_ref         0.3628
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5089
_reflns_number_total             7711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00650b11.cif
_cod_data_source_block           ac500
_cod_database_code               7709853
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F45-P6
 1.56 with sigma of 0.02
 F12-F3 = F45-F8
 2.2 with sigma of 0.02
 F33-F45
 2.2 with sigma of 0.02
 F38-F45
 2.2 with sigma of 0.02
 F45-F7
 2.2 with sigma of 0.02
 P6-F45
 1.56 with sigma of 0.02
 B6A-F45A
 1.48 with sigma of 0.02
 F8A-B6A
 1.48 with sigma of 0.02
 F22A-B6A
 1.48 with sigma of 0.02
 F7A-B6A
 1.48 with sigma of 0.02
 F45A-F8A
 2.25 with sigma of 0.02
 F7A-F45A
 2.25 with sigma of 0.02
 F45A-F22A
 2.25 with sigma of 0.02
 P6-F7 \\sim B6A-F7A
 with sigma of 0.02
 P6-F8 \\sim B6A-F8A
 with sigma of 0.02
 P6-F22 \\sim B6A-F22A
 with sigma of 0.02
 P6-F45 \\sim B6A-F45A
 with sigma of 0.02
 F7-F8 \\sim F7A-F8A
 with sigma of 0.04
 F7-F22 \\sim F7A-F22A
 with sigma of 0.04
 F7-F45 \\sim F7A-F45A
 with sigma of 0.04
 F8-F22 \\sim F8A-F22A
 with sigma of 0.04
 F8-F45 \\sim F8A-F45A
 with sigma of 0.04
 F22-F45 \\sim F22A-F45A
 with sigma of 0.04
 P1-F3 \\sim P1A-F3A
 with sigma of 0.02
 P1-F9 \\sim P1A-F9A
 with sigma of 0.02
 P1-F2 \\sim P1A-F2A
 with sigma of 0.02
 P1-F6 \\sim P1A-F6A
 with sigma of 0.02
 P1-F1 \\sim P1A-F1A
 with sigma of 0.02
 P1-F12 \\sim P1A-F12A
 with sigma of 0.02
 F3-F9 \\sim F3A-F9A
 with sigma of 0.04
 F3-F2 \\sim F3A-F2A
 with sigma of 0.04
 F3-F6 \\sim F3A-F6A
 with sigma of 0.04
 F3-F1 \\sim F3A-F1A
 with sigma of 0.04
 F3-F12 \\sim F3A-F12A
 with sigma of 0.04
 F9-F2 \\sim F9A-F2A
 with sigma of 0.04
 F9-F6 \\sim F9A-F6A
 with sigma of 0.04
 F9-F1 \\sim F9A-F1A
 with sigma of 0.04
 F9-F12 \\sim F9A-F12A
 with sigma of 0.04
 F2-F6 \\sim F2A-F6A
 with sigma of 0.04
 F2-F1 \\sim F2A-F1A
 with sigma of 0.04
 F2-F12 \\sim F2A-F12A
 with sigma of 0.04
 F6-F1 \\sim F6A-F1A
 with sigma of 0.04
 F6-F12 \\sim F6A-F12A
 with sigma of 0.04
 F1-F12 \\sim F1A-F12A
 with sigma of 0.04
 P4-C27 \\sim P4-C27A
 with sigma of 0.02
 C27-C53 \\sim C27A-C53A
 with sigma of 0.02
 C27-C47 \\sim C27A-C47A
 with sigma of 0.02
 C53-C44 \\sim C53A-C44A
 with sigma of 0.02
 C44-C23 \\sim C44A-C23A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C24-C47 \\sim C24A-C47A
 with sigma of 0.02
 P4-C53 \\sim P4-C53A
 with sigma of 0.04
 P4-C47 \\sim P4-C47A
 with sigma of 0.04
 C27-C44 \\sim C27A-C44A
 with sigma of 0.04
 C27-C24 \\sim C27A-C24A
 with sigma of 0.04
 C53-C23 \\sim C53A-C23A
 with sigma of 0.04
 C53-C47 \\sim C53A-C47A
 with sigma of 0.04
 C44-C24 \\sim C44A-C24A
 with sigma of 0.04
 C23-C47 \\sim C23A-C47A
 with sigma of 0.04
 P4-C28 \\sim P4-C28A
 with sigma of 0.02
 C28-C32 \\sim C28A-C32A
 with sigma of 0.02
 C28-C36 \\sim C28A-C36A
 with sigma of 0.02
 C32-C57 \\sim C32A-C57A
 with sigma of 0.02
 C57-C61 \\sim C57A-C61A
 with sigma of 0.02
 C61-C51 \\sim C61A-C51A
 with sigma of 0.02
 C51-C36 \\sim C51A-C36A
 with sigma of 0.02
 P4-C32 \\sim P4-C32A
 with sigma of 0.04
 P4-C36 \\sim P4-C36A
 with sigma of 0.04
 C28-C57 \\sim C28A-C57A
 with sigma of 0.04
 C28-C51 \\sim C28A-C51A
 with sigma of 0.04
 C32-C61 \\sim C32A-C61A
 with sigma of 0.04
 C32-C36 \\sim C32A-C36A
 with sigma of 0.04
 C57-C51 \\sim C57A-C51A
 with sigma of 0.04
 C61-C36 \\sim C61A-C36A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C28A) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C27A) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(P1A) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(P1) = Uanis(F3) = Uanis(F2) = Uanis(F9) = Uanis(F1) = Uanis(F6) =
Uanis(F12)
Uanis(B6A) = Uanis(F22A) = Uanis(F7A) = Uanis(F8A) = Uanis(F45A)
Uanis(P1A) = Uanis(F3A) = Uanis(F6A) = Uanis(F12A) = Uanis(F1A) = Uanis(F9A) =
Uanis(F2A)
Uanis(P6) = Uanis(F7) = Uanis(F8) = Uanis(F22) = Uanis(F33) = Uanis(F38) =
Uanis(F45)
Uanis(C27) = Uanis(C47) = Uanis(C24) = Uanis(C23) = Uanis(C44) = Uanis(C53)
Uanis(C28) = Uanis(C32) = Uanis(C57) = Uanis(C61) = Uanis(C51) = Uanis(C36)
Uanis(C27A) = Uanis(C53A) = Uanis(C44A) = Uanis(C23A) = Uanis(C24A) =
Uanis(C47A)
Uanis(C28A) = Uanis(C32A) = Uanis(C57A) = Uanis(C61A) = Uanis(C51A) =
Uanis(C36A)
Uanis(P4) = Uanis(C27A)
Uanis(P4) = Uanis(C27)
Uanis(P4) = Uanis(C28A)
Uanis(P4) = Uanis(C28)
4. Others
 Sof(F22A)=Sof(B6A)=Sof(F7A)=Sof(F8A)=Sof(F45A)=1-FVAR(1)
 Sof(P6)=Sof(F7)=Sof(F8)=Sof(F22)=Sof(F33)=Sof(F38)=Sof(F45)=FVAR(1)
 Sof(P1A)=Sof(F6A)=Sof(F1A)=Sof(F9A)=Sof(F3A)=Sof(F2A)=Sof(F12A)=1-FVAR(2)
 Sof(P1)=Sof(F3)=Sof(F9)=Sof(F2)=Sof(F6)=Sof(F1)=Sof(F12)=FVAR(2)
 Sof(C27A)=Sof(C53A)=Sof(H53A)=Sof(C44A)=Sof(H44A)=Sof(C23A)=Sof(H23A)=
 Sof(C24A)=Sof(H24A)=Sof(C47A)=Sof(H47A)=1-FVAR(3)
 Sof(C27)=Sof(C53)=Sof(H53)=Sof(C44)=Sof(H44)=Sof(C23)=Sof(H23)=Sof(C24)=
 Sof(H24)=Sof(C47)=Sof(H47)=FVAR(3)
 Sof(C28A)=Sof(C32A)=Sof(H32A)=Sof(C57A)=Sof(H57A)=Sof(C61A)=Sof(H61A)=
 Sof(C51A)=Sof(H51A)=Sof(C36A)=Sof(H36A)=1-FVAR(4)
 Sof(C28)=Sof(C32)=Sof(H32)=Sof(C57)=Sof(H57)=Sof(C61)=Sof(H61)=Sof(C51)=
 Sof(H51)=Sof(C36)=Sof(H36)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C15(H15)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C21(H21), C53(H53), C44(H44), C23(H23), C24(H24), C47(H47),
 C32(H32), C57(H57), C61(H61), C51(H51), C36(H36), C17(H17), C10(H10), C25(H25),
  C18(H18), C48(H48), C39(H39), C43(H43), C19(H19), C22(H22), C20(H20), C6(H6),
 C16(H16), C9(H9), C2(H2), C1(H1), C13(H13), C3(H3), C4(H4), C8(H8), C5(H5),
 C53A(H53A), C44A(H44A), C23A(H23A), C24A(H24A), C47A(H47A), C32A(H32A),
 C57A(H57A), C61A(H61A), C51A(H51A), C36A(H36A)
5.c Fitted hexagon refined as free rotating group:
 C27(C53,C44,C23,C24,C47), C28(C32,C57,C61,C51,C36), C27A(C53A,C44A,C23A,C24A,
 C47A), C28A(C32A,C57A,C61A,C51A,C36A)
;
_olex2_submission_special_instructions 'No special instructions were received'