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_7719650
_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         'C70 H116 O4 Tm2'
_chemical_formula_sum            'C48 H47 N2 P3'
_chemical_formula_weight         744.78
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-04-10
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-07-31 deposited with the CCDC.	2025-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.478(4)
_cell_angle_beta                 90.470(4)
_cell_angle_gamma                100.039(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9376(5)
_cell_length_b                   12.5643(6)
_cell_length_c                   14.6202(7)
_cell_measurement_reflns_used    24609
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.87
_cell_measurement_theta_min      2.17
_cell_volume                     1978.23(16)
_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_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M CDTE'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_details      '304 frames, detector distance = 70 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  0.0317
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21360
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.215
_diffrn_reflns_theta_min         2.167
_diffrn_source                   Axo_Mo
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.9910
_exptl_absorpt_correction_T_min  0.9910
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         9385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0555
_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^)+(0.0585P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6798
_reflns_number_total             9385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02099a2.cif
_cod_data_source_block           ip3-57
_cod_depositor_comments
'Adding full bibliography for 7719650--7719651.cif.'
_cod_database_code               7719650
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.972
_diffrn_oxdiff_ac3_digest_hkl    0168e077c0e1f9f92b3a4aa5d07df000c06de4
_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.a Ternary CH refined with riding coordinates:
 C00V(H00V), C00Z(H00Z)
2.b Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00D(H00D), C00E(H00E), C00G(H00G), C00H(H00H), C00I(H00I),
 C00K(H00K), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00W(H00W), C00X(H00X),
 C00Y(H00Y), C010(H010), C011(H011), C012(H012), C013(H013), C014(H014),
 C015(H015), C016(H016), C017(H017), C018(H018), C019(H019), C01A(H01A),
 C01B(H01B), C01D(H01F), C01F(H01J)
2.c Idealised Me refined as rotating group:
 C01C(H01C,H01D,H01E), C01E(H01G,H01H,H01I), C01G(H01K,H01L,H01M), C01H(H01N,
 H01O,H01P)
;
_shelx_res_checksum              60893
_shelx_hkl_checksum              43840
_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 -
_stoe_evaluation_lana_bos_l_odd_max -
_stoe_evaluation_lana_completeness 87.4
_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 21362
_stoe_evaluation_lana_number_refls_outliers 1083
_stoe_evaluation_lana_number_refls_total 22445
_stoe_evaluation_lana_number_refls_unique 9387
_stoe_evaluation_lana_number_refls_written 21362
_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 -1
_stoe_evaluation_lana_table
;
2Theta           6.6   12.8   19.0   25.2   31.4   37.6   43.8   50.0   56.2
<Resolution>    5.14   3.12   2.17   1.61   1.31   1.10   0.95   0.84   0.77
N(total)         307    987   1374   2082   3088   3951   4397   4576   1683
<Redundancy>     4.7    4.7    3.1    2.8    2.7    2.5    2.2    1.9    1.4
Complet. [%%]   100.0  100.0   97.3   99.1   99.7   99.8   99.5   99.1   48.0
<I/sigma>      150.7   80.6   49.8   25.9   18.4   10.9    6.8    4.4    2.8
R(int)         0.020  0.020  0.023  0.026  0.031  0.037  0.056  0.073  0.094
;
_stoe_measurement_identifier     ip3-57
_stoe_measurement_max_exposure_per_frame '5.0 s'
_stoe_measurement_mean_exposure_per_frame '5.0 s'
_stoe_measurement_min_exposure_per_frame '5.0 s'
_stoe_measurement_total_exposure_time '55 min'
_stoe_measurement_total_frame_number 654
_stoe_measurement_total_run_number 12
_stoe_measurement_tube_power     '50.0 W'