Unusual cleavage of phosphaalkynes triple bond in the coordination sphere of transition metals
Moussa, Mehdi; Rummel, Eva-Maria; Eckhardt, Maria; Riesinger, Christoph; Scheer, Manfred; Dalton Transactions  (2023) –; doi:10.1039/D3DT02472E

data_7714186
_publ_section_title
;
 Unusual cleavage of phosphaalkynes triple bond in the coordination sphere
 of transition metals
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02472E
_journal_year                    2023
_chemical_formula_moiety         'C18 H9 Fe4 O13 P1'
_chemical_formula_sum            'C18 H9 Fe4 O13 P'
_chemical_formula_weight         687.62
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-03-01
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.01.27 svn.rdd5efbe3 for OlexSys, GUI svn.r6708)
;
_audit_update_record
;
2023-07-16 deposited with the CCDC.	2023-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   8.7479(4)
_cell_length_b                   8.7479(4)
_cell_length_c                   54.779(3)
_cell_measurement_reflns_used    3922
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      76.5220
_cell_measurement_theta_min      4.8398
_cell_volume                     3630.4(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      123.0(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -75.00   38.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564   77.0000   60.0000 113

  2 omega  -72.00   38.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564   77.0000  -60.0000 110

  3 omega  -75.00   38.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564   77.0000 -180.0000 113

  4 omega   77.00  140.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -80.0000  -42.0000 63

  5 omega   65.00  124.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -80.0000  174.0000 59

  6 omega   82.00  126.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   77.0000 -150.0000 44

  7 omega   33.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -80.0000  174.0000 27

  8 omega   85.00  154.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  -90.0000 69

  9 omega   85.00  152.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  150.0000 67

 10 omega   86.00  158.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000    0.0000 72

 11 omega   89.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  120.0000 27

 12 omega  127.00  156.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000  120.0000 29

 13 omega   38.00  144.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -80.0000   77.0000 106

 14 omega   33.00   59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -80.0000  -42.0000 26

 15 omega   41.00   77.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -45.0000 -120.0000 36

 16 omega   85.00  149.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   45.0000   60.0000 64

 17 omega   69.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000  -80.0000  -94.0000 78
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       67
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            6850
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.722
_diffrn_reflns_theta_min         4.844
_exptl_absorpt_coefficient_mu    20.073
_exptl_absorpt_correction_T_max  0.290
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_description       block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.478
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 727 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1623
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0971P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                1575
_reflns_number_total             1623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02472e2.cif
_cod_data_source_block           rue016
_cod_original_cell_volume        3630.4(4)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               7714186
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              59078
_olex2_submission_special_instructions 'No special instructions were received'