Catalytic olefin hydrosilylation with an original bis(iminophosphorane)phosphine NPN Co<sup>II</sup> complex.
Popovici, Ingrid; Chen, Yujia; Bourcier, Sophie; Casaretto, Nicolas; Auffrant, Audrey; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15705–15709; doi:10.1039/d5dt02099a

data_7719651
_publ_section_title
;
 Catalytic olefin hydrosilylation with an original
 bis(iminophosphorane)phosphine NPN Co<sup>II</sup> complex.
;
_journal_issue                   42
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15705
_journal_page_last               15709
_journal_paper_doi               10.1039/d5dt02099a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C48 H47 Br0.257 Cl0.743 Co N2 P3, F6 P'
_chemical_formula_sum            'C48 H47 Br0.26 Cl0.74 Co F6 N2 P4'
_chemical_formula_weight         995.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-06-18
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.22 svn.r631f81ec for OlexSys, GUI svn.r7248)
;
_audit_update_record
;
2025-07-31 deposited with the CCDC.	2025-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.761(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1288(6)
_cell_length_b                   31.464(2)
_cell_length_c                   14.1400(8)
_cell_measurement_reflns_used    13050
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.80
_cell_measurement_theta_min      2.13
_cell_volume                     4475.0(5)
_computing_cell_refinement
;
X-Area Recipe 2.0.2 (STOE, 2024)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.194.0 (STOE, 2023)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
 340 frames, detector distance = 60 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19855
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.403
_diffrn_source                   Axo_Mo
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_T_max  0.9074
_exptl_absorpt_correction_T_min  0.8241
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'greenish blue'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2047
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0405P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0850
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5040
_reflns_number_total             7815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02099a2.cif
_cod_data_source_block           ip3-161
_cod_depositor_comments
'Adding full bibliography for 7719650--7719651.cif.'
_cod_database_code               7719651
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.836
_diffrn_oxdiff_ac3_digest_hkl    011f3cb4ebe0d47c214ff40f072c0ad8ed855f
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{Cl8, Br1}
3. Uiso/Uaniso restraints and constraints
Uanis(Cl8) = Uanis(Br1)
4. Others
 Sof(Br1)=1-FVAR(1)
 Sof(Cl8)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C00R(H00R), C00W(H00W)
5.b Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00J(H00J), C00K(H00K), C00N(H00N), C00O(H00O), C00P(H00P),
 C00Q(H00Q), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V), C00X(H00X),
 C00Z(H00Z), C011(H011), C014(H014), C015(H015), C016(H016), C017(H017),
 C018(H018), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D),
 C01G(H01K), C01H(H01L), C01I(H01M), C01K(H01Q), C01M(H01U), C01N(H01V),
 C01O(H01W), C01P(H01X), C01Q(H01Y)
5.c Idealised Me refined as rotating group:
 C01E(H01E,H01F,H01G), C01F(H01H,H01I,H01J), C01J(H01N,H01O,H01P), C01L(H01R,
 H01S,H01T)
;
_shelx_res_checksum              11612
_shelx_hkl_checksum              69432
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '60.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   10.1
_stoe_evaluation_integration_b   0.1
_stoe_evaluation_integration_ems 0.011
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 6
_stoe_evaluation_lana_bos_l_odd_max 3
_stoe_evaluation_lana_completeness 85.6
_stoe_evaluation_lana_dxs_max_order 3
_stoe_evaluation_lana_dys_max_order 3
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 58.5
_stoe_evaluation_lana_max_2theta_desired 58.5
_stoe_evaluation_lana_mean_redundancy 2.3
_stoe_evaluation_lana_number_refls_after_or 23954
_stoe_evaluation_lana_number_refls_outliers 841
_stoe_evaluation_lana_number_refls_total 24795
_stoe_evaluation_lana_number_refls_unique 10607
_stoe_evaluation_lana_number_refls_written 23954
_stoe_evaluation_lana_or_c1      0.050
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      1.0
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
2Theta           6.8   13.0   19.2   25.4   31.6   37.8   44.0   50.2   56.4
<Resolution>    5.05   3.07   2.14   1.60   1.30   1.09   0.95   0.84   0.77
N(total)         389   1191   1649   2550   3775   4538   4761   4450   1492
<Redundancy>     5.0    4.7    3.1    2.9    2.9    2.6    2.1    1.7    1.3
Complet. [%%]    98.6   99.1   98.8   99.9   99.4   99.5   98.6   95.1   42.7
<I/sigma>       70.9   42.8   26.3   17.3    8.9    5.1    2.9    1.5    1.0
R(int)         0.018  0.019  0.022  0.026  0.042  0.067  0.105  0.183  0.242
;
_stoe_measurement_identifier     IP3-161
_stoe_measurement_max_exposure_per_frame '45.0 s'
_stoe_measurement_mean_exposure_per_frame '45.0 s'
_stoe_measurement_min_exposure_per_frame '45.0 s'
_stoe_measurement_total_exposure_time '4.2 h'
_stoe_measurement_total_frame_number 340
_stoe_measurement_total_run_number 7
_stoe_measurement_tube_power     '50.0 W'