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_1572869
_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         'C60 H90 N2 O5 P2 Si2 W, 5(C6 H6)'
_chemical_formula_sum            'C90 H120 N2 O5 P2 Si2 W'
_chemical_formula_weight         1611.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2024-07-11 deposited with the CCDC.	2024-10-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.772(2)
_cell_length_b                   18.812(2)
_cell_length_c                   31.181(4)
_cell_measurement_reflns_used    9460
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3435
_cell_measurement_theta_min      2.186
_cell_volume                     8664.9(19)
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'Bruker Photon III C7 CMOS'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            205991
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.341
_diffrn_reflns_theta_min         1.264
_diffrn_source                   'Incoatec Microsource'
_exptl_absorpt_coefficient_mu    1.447
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_correction_T_min  0.343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       block
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.692
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 9255 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0057(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1259
_refine_ls_number_reflns         21441
_refine_ls_number_restraints     5608
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+1.9356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0504
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                20928
_reflns_number_total             21441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc05491a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1572866--1572869.cif.'
_cod_database_code               1572869
_shelx_shelxl_version_number     2019/1
_shelx_res_checksum              26983
_shelx_hkl_checksum              60842