Phosphasilene mediated CO activation and deoxygenative homo coupling of CO molecules in reactions with metal carbonyls.
Hendi, Zohreh; Pradhan, Renuka; Rachuy, Katharina; Mahmoudi, Soheil; Pandey, Madhusudan K.; Kushvaha, Saroj Kumar; Herbst-Irmer, Regine; Lourderaj, Upakarasamy; Stalke, Dietmar; Roesky, Herbert W.; Chemical science 15 (2024) 18888–18895; doi:10.1039/d4sc05491a

data_1572866
_publ_section_title
;
 Phosphasilene mediated CO activation and deoxygenative homo coupling of
 CO molecules in reactions with metal carbonyls.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              18888
_journal_page_last               18895
_journal_paper_doi               10.1039/d4sc05491a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C59 H90 Fe N2 O4 P2 Si2)'
_chemical_formula_sum            'C118 H180 Fe2 N4 O8 P4 Si4'
_chemical_formula_weight         2130.59
_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             2023-07-04
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-04 deposited with the CCDC.	2024-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                89.148(4)
_cell_angle_beta                 68.098(4)
_cell_angle_gamma                69.912(4)
_cell_formula_units_Z            1
_cell_length_a                   13.3341(7)
_cell_length_b                   15.4736(9)
_cell_length_c                   16.8028(9)
_cell_measurement_reflns_used    36730
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.83
_cell_measurement_theta_min      3.17
_cell_volume                     2995.3(3)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1050
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            102143
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         2.534
_diffrn_source                   'Axo Mo'
_exptl_absorpt_coefficient_mu    0.390
_exptl_absorpt_correction_T_max  0.9840
_exptl_absorpt_correction_T_min  0.9333
_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.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.237
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         11773
_refine_ls_number_restraints     1170
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0585
_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^)+(0.1700P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9426
_reflns_number_total             11773
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05491a2.cif
_cod_data_source_block           fepsi
_cod_depositor_comments
'Adding full bibliography for 1572866--1572869.cif.'
_cod_database_code               1572866
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.892
_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. Restrained distances
 C22-C40 \\sim C22-C40A
 with sigma of 0.02
 C40-C41 \\sim C40A-C41A
 with sigma of 0.02
 C40-C52 \\sim C40A-C52A
 with sigma of 0.02
 C40-C53 \\sim C40A-C53A
 with sigma of 0.02
 C22-C41 \\sim C22-C41A
 with sigma of 0.04
 C22-C52 \\sim C22-C52A
 with sigma of 0.04
 C22-C53 \\sim C22-C53A
 with sigma of 0.04
 C41-C52 \\sim C41A-C52A
 with sigma of 0.04
 C41-C53 \\sim C41A-C53A
 with sigma of 0.04
 C52-C53 \\sim C52A-C53A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C53A)=Sof(H53D)=Sof(H53E)=Sof(H53F)=Sof(C40A)=Sof(C52A)=Sof(H52D)=
 Sof(H52E)=Sof(H52F)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(1)
 Sof(C40)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(C52)=Sof(H52A)=Sof(H52B)=
 Sof(H52C)=Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=FVAR(1)
6.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C21(H21), C23(H23), C27(H27), C29(H29)
6.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C),
 C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C61(H61A,H61B,H61C), C53A(H53D,H53E,H53F), C52A(H52D,H52E,H52F),
 C41A(H41D,H41E,H41F)
;
_shelx_res_checksum              19338
_shelx_hkl_checksum              96809
_olex2_submission_original_sample_id FEPSI
_olex2_submission_special_instructions 'No special instructions were received'